阅读说明：本技术 溶液处理装置和溶液处理方法 (Function Solution Handling Device Used and solution processing methods ) 是由 小田昭昌 铃木崇夫 石泽英树 增田义登 宝木雅人 清水巧治 于 2018-11-02 设计创作，主要内容包括：本发明的课题在于,提供即使被处理液的不挥发性成分析出也能够发挥优异的处理效率的溶液处理装置和溶液处理方法。本发明的溶液处理装置(1A)的特征在于,其具备：第1气液分离单元(10),其将被处理液(L1)加热、使蒸气馏出并且使所保持的浓缩液的一部分出罐；第2气液分离单元(20),其将从前述第1气液分离单元(10)出罐的浓缩液加热、使蒸气馏出并且使所保持的浓缩液的一部分出罐；以及,控制单元(30),其控制前述第1气液分离单元(10),以使在前述第1气液分离单元(10)中被处理液(L1)中含有的不挥发性成分不析出,前述第2气液分离单元(20)的作为将浓缩液加热的部位且与浓缩液接触的接液部位对不挥发性成分呈耐附着性。(Problem of the present invention is that providing even if the fixedness of liquid to be treated into the Function Solution Handling Device Used and solution processing methods that can play excellent treatment effeciency analyzing.Function Solution Handling Device Used (1A) of the invention is characterized in that having: the 1st gas-liquid separation unit (10), by liquid to be treated (L1) heating, distillates steam and a part of kept concentrate is made to go out tank；2nd gas-liquid separation unit (20) by the concentrate for going out tank from aforementioned 1st gas-liquid separation unit (10) heating, distillates steam and a part of kept concentrate is made to go out tank；And, control unit (30), it controls aforementioned 1st gas-liquid separation unit (10), so that the fixedness ingredient contained in liquid to be treated (L1) in aforementioned 1st gas-liquid separation unit (10) is not precipitated, the liquid position that connects of aforementioned 2nd gas-liquid separation unit (20) contacted as the position for heating concentrate and with concentrate is in resistance to adhesion to fixedness ingredient.)

1. a kind of Function Solution Handling Device Used, which is characterized in that the Function Solution Handling Device Used from contain organic solvent and fixedness ingredient Liquid to be treated in organic solvent is separated in the form of distillating steam, which has:

1st gas-liquid separation unit by liquid to be treated heating, distillates steam and goes out a part of kept concentrate Tank；

2nd gas-liquid separation unit, by the concentrate for going out tank from the 1st gas-liquid separation unit heating, make steam distillate and A part of kept concentrate is set to go out tank；And

Control unit controls the 1st gas-liquid separation unit, so that in the 1st gas-liquid separation unit in liquid to be treated The fixedness ingredient contained is not precipitated,

2nd gas-liquid separation unit contacted as the position for heating concentrate and with concentrate connect liquid position to not waving Hair property ingredient is in resistance to adhesion.

2. Function Solution Handling Device Used according to claim 1, which is characterized in that it has with regulation flow velocity conveying the described 2nd The pump of the concentrate of the inside of gas-liquid separation unit,

Described control unit controls the pump, so that the regulation flow velocity is the stream that accumulates fixedness ingredient be precipitated Speed.

3. Function Solution Handling Device Used according to claim 1 or 2, which is characterized in that described control unit controls the 1st gas Liquid separative unit distillates rate so that its be start to be precipitated than the fixedness ingredient that contains in liquid to be treated to distillate rate low Distillate rate.

4. Function Solution Handling Device Used described in any one of claim 1 to 3, which is characterized in that described control unit is with such as Under mode controlled: reach predetermined temperature in the liquid temperature for meeting the concentrate that the 2nd gas-liquid separation unit is kept In at the time of the amount for the concentrate that moment and the 2nd gas-liquid separation unit are kept reaches specified amount at least 1 when It carves, so that concentrate is gone out tank until the concentrate that the 2nd gas-liquid separation unit is kept reaches specified amount.

5. Function Solution Handling Device Used according to any one of claims 1 to 4, which is characterized in that serve as reasons at the liquid position that connects The coating state of the material of resistance to adhesion or surface roughness are 1 μm of state below.

6. a kind of solution processing methods, which is characterized in that the solution processing methods from contain organic solvent and fixedness ingredient Liquid to be treated in organic solvent is separated in the form of distillating steam, this method comprises:

1st gas-liquid separation process by liquid to be treated heating, distillates steam and goes out a part of kept concentrate Tank；And

2nd gas-liquid separation process by the concentrate heating for going out tank in the 1st gas-liquid separation process, makes steam distillate and make A part of the concentrate kept goes out tank,

In the 1st gas-liquid separation process, it is controlled such that the fixedness ingredient contained in liquid to be treated is not precipitated,

In the 2nd gas-liquid separation process, what is contacted as the position for heating concentrate and with concentrate connects liquid position pair Fixedness ingredient is in resistance to adhesion.

7. solution processing methods according to claim 6, which is characterized in that, will be dense in the 2nd gas-liquid separation process The flow velocity of contracting liquid is set as the flow velocity for accumulating fixedness ingredient be precipitated.

8. solution processing methods according to claim 6 or 7, which is characterized in that make in the 1st gas-liquid separation process Distillate rate be start to be precipitated than the fixedness ingredient that contains in liquid to be treated distillate rate it is low distillate rate.

9. the solution processing methods according to any one of claim 6~8, which is characterized in that in the 2nd gas-liquid separation In process, at the time of the liquid temperature for meeting kept concentrate reaches predetermined temperature and the amount of concentrate that is kept reaches In at the time of specified amount at least 1 at the time of, so that concentrate is gone out tank until the concentrate that is kept reaches specified amount.

10. the solution processing methods according to any one of claim 6~9, which is characterized in that serve as reasons at the liquid position that connects The coating state of the material of resistance to adhesion or surface roughness are 1 μm of state below.

Technical field

The present invention relates to separate organic solvent from the liquid to be treated for being mixed with fixedness ingredient in organic solvent Function Solution Handling Device Used and solution processing methods.

Background technique

There is the purposes of the lytic agent for dissolving the objects such as resin, the dispersing agent for dispersing it in organic solvent.In addition, having Solvent crystal liquid substrate, semiconductor integrated circuit manufacturing process in also as be referred to as photoresist photoresist Remover use.

Moreover, the organic solvent used in this purposes can remove impurity in most cases and be recycled, for The recycling of organic solvent, commonly used this impurity separation method of distillation.

About the technology for recycling organic solvent by distillation, propose in various technologies, such as patent document 1 Disclose a kind of resist regeneration method, which is characterized in that it has: by the resist being discharged from resist apparatus for coating with have The process of the mixed liquor recycling of solvent；The process that aforementioned organic solvents volatilization is concentrated by aforementioned mixed liquor；It will be volatilized The liquefied process of aforementioned organic solvents；And by the way that aforementioned concentration mixed liquor is added by aforementioned mixed liquor in organic solvent Viscosity-adjusting agent to desired value process.

Summary of the invention

Problems to be solved by the invention

However, as disclosed in Patent Document 1 there are the fixednesies such as the resin of dissolution in organic solvent in existing method At the attachment of fixedness ingredient (fixed, adherency etc.) the connecing in the evaporator for evaporating organic solvent for analyzing, being precipitated The anxiety at liquid position.As a result, existing method can generate the heating properties of evaporator through when reduction, can not play and to improve solvent The rate of recovery prevents heat-insulated loss in pipeline, energy conservation these effects for being expected.

As countermeasure for this problem, it can enumerate and carry out organic solvent under conditions of fixedness ingredient is not precipitated The method of detached job, the countermeasure is since the treatment effeciency (distillating rate) of organic solvent is deteriorated, and the amount of waste increases, because This is not also referred to as preferred method economically, environmentally.

Therefore, it problem of the present invention is that, provides excellent at that can be played analyzing even if the fixedness of liquid to be treated The Function Solution Handling Device Used and solution processing methods of different treatment effeciency.

The solution to the problem

As the means for solving aforementioned problems, Function Solution Handling Device Used of the invention is characterized in that, solution processing Device separates organic solvent from the liquid to be treated containing organic solvent and fixedness ingredient in the form of distillating steam, should Device has: the 1st gas-liquid separation unit, by liquid to be treated heating, distillates steam and makes the one of kept concentrate Part goes out tank；2nd gas-liquid separation unit by the concentrate for going out tank from aforementioned 1st gas-liquid separation unit heating, distillates steam And a part of kept concentrate is made to go out tank；And control unit, aforementioned 1st gas-liquid separation unit is controlled, so that The fixedness ingredient contained in liquid to be treated in aforementioned 1st gas-liquid separation unit is not precipitated, aforementioned 2nd gas-liquid separation unit Contacted as the position for heating concentrate and with concentrate connect liquid position to fixedness ingredient in resistance to adhesion.

In addition, solution processing methods of the invention are characterized in that, the solution processing methods are from containing organic solvent and not Organic solvent is separated in the form of distillating steam in the liquid to be treated of volatile component, this method comprises: the 1st gas-liquid separation work Sequence by liquid to be treated heating, distillates steam and a part of kept concentrate is made to go out tank；And the 2nd gas-liquid separation Process by the concentrate heating for going out tank in aforementioned 1st gas-liquid separation process, distillates steam and makes kept concentrate A part goes out tank and is controlled such that the fixedness ingredient contained in liquid to be treated not in aforementioned 1st gas-liquid separation process It is precipitated, in aforementioned 2nd gas-liquid separation process, what is contacted as the position for heating concentrate and with concentrate connects liquid position pair Fixedness ingredient is in resistance to adhesion.

The effect of invention

In accordance with the invention it is possible to provide even if the fixedness of liquid to be treated at excellent processing can be played analyzing The Function Solution Handling Device Used and solution processing methods of efficiency.

Detailed description of the invention

Fig. 1 is the schematic diagram of the Function Solution Handling Device Used of present embodiment.

Fig. 2 is the schematic diagram of the Function Solution Handling Device Used of variation.

Fig. 3 A is the table for showing result obtained in the trial test of embodiment 1.

Fig. 3 B is the chart of concentrate temperature and fixedness constituent concentration obtained in the trial test of embodiment 1.

Fig. 3 C is concentrate temperature obtained in the trial test of embodiment 1 and the chart for distillating rate.

Fig. 4 A is the table for showing result obtained in the trial test of embodiment 3.

Fig. 4 B is the chart of concentrate temperature and fixedness constituent concentration obtained in the trial test of embodiment 3.

Fig. 4 C is concentrate temperature obtained in the trial test of embodiment 3 and the chart for distillating rate.

Specific embodiment

Hereinafter, suitably referring to attached drawing to embodiment (this reality of Function Solution Handling Device Used and solution processing methods of the invention Apply mode) it is illustrated.

Firstly, being illustrated referring to Fig.1 to the overview of the Function Solution Handling Device Used of present embodiment.

" overview of the Function Solution Handling Device Used of present embodiment "

The Function Solution Handling Device Used 1A of present embodiment is from the liquid to be treated L1 containing organic solvent and fixedness ingredient The middle device for separating organic solvent in the form of distillating steam G4.

Then, as shown in Figure 1, Function Solution Handling Device Used 1A have the 1st gas-liquid separation unit 10 (the 1st gas-liquid separation container 11, 1st evaporator 12), the 2nd gas-liquid separation unit 20 (the 2nd gas-liquid separation container 21, the 2nd evaporator 22) and control unit 30.

In addition, being connected (with outside) by being piped t1~t11 between each component of Function Solution Handling Device Used 1A, and in order to adjust this The flowing of the solution (liquid to be treated, concentrate) of the inside of a little pipings and each component and have pump P1, P2, valve V1~5.

In addition, Function Solution Handling Device Used 1A has solid removal unit 40, and have flowmeter F1~F4, liquidometer S1, S2, thermometer T1, T2 these metrical instruments.

Then, each component of the Function Solution Handling Device Used 1A of present embodiment is illustrated referring to Fig.1.

<the 1st gas-liquid separation unit>

1st gas-liquid separation unit 10 is by liquid to be treated L1 heating, distillates steam and make kept concentrate A part goes out the unit of tank.

Moreover, the 1st gas-liquid separation unit 10 includes the 1st gas-liquid separation container 11 and the 1st evaporator 12 and constitutes.

It should be noted that in the 1st gas-liquid separation unit 10, so that the fixedness ingredient contained in liquid to be treated is not The mode of precipitation is implemented to control, and detailed control method is described in detail below.

(the 1st gas-liquid separation container)

1st gas-liquid separation container 11 will pass through the liquid to be treated L1 of piping t1 supply, pass through the steaming of piping t4 and t9 supply The concentrate and then the concentrate by being piped t4 supply that gas G1 and G3 is condensed in aftermentioned gas-liquid separator 13 and flowed down exist The bottom of container keeps specified amount, and them is made to go out tank from bottom with defined flow.

In addition, the 1st gas-liquid separation container 11 make by piping t4 and t9 supply steam G1 and G3 in, in aftermentioned gas It has carried out distillating at the top of the vapors from vessel of gas-liquid separation in liquid/gas separator 13, sent as steam G4 is distillated by being piped t10 Outside is arrived out.

Also, in the 1st gas-liquid separation container 11, container inside and than be piped t1, t4, t9 connecting portion it is top Position be provided with gas-liquid separator 13, and being provided with to the concentrate of the bottom for being maintained at container (also includes liquid to be treated L1 the liquidometer S1 that the height of liquid level) the measures and thermometer T1 that the temperature of concentrate is measured.

It should be noted that, although the 1st gas-liquid separation container 11 is in tower-like in Fig. 1, but shape is not particularly limited, For size, also suitably set according to treating capacity of liquid to be treated L1 etc..

As long as in addition, gas-liquid separator 13 can from gas by liquid separate equipment be not particularly limited, example As can be using gas-liquid separator equipment well known to these of demister, cyclone separating.

(the 1st evaporator)

1st evaporator 12 will go out tank from the 1st gas-liquid separation container 11, be heated and steamed by the concentrate that piping t2, t3 are supplied Hair.Then, generated steam G1 and heated concentrate are supplied to the 1st gas-liquid separation by being piped t4 by the 1st evaporator 12 Container 11.

It should be noted that as long as the equipment that concentrate can be heated and be evaporated by the 1st evaporator 12 is then without special It limits, it can be using multitube, board-like, jacket type, coiled, double hose these various forms of heat exchangers etc..Moreover, being Blocking etc. is prevented, filter preferably is set in the upstream side of the 1st evaporator 12 or downstream side.

<the 2nd gas-liquid separation unit>

2nd gas-liquid separation unit 20 is will to go out the concentrate heating of tank from the 1st gas-liquid separation unit 10, distillate steam simultaneously And a part of kept concentrate is made to go out the unit of tank.

Moreover, the 2nd gas-liquid separation unit 20 includes the 2nd gas-liquid separation container 21 and the 2nd evaporator 22 and constitutes.

(the 2nd gas-liquid separation container)

2nd gas-liquid separation container 21 is by the concentrate supplied by piping t5 from the 1st gas-liquid separation container 11 in container Bottom keeps specified amount, and it is made to go out tank from bottom with defined flow.

In addition, the 2nd gas-liquid separation container 21 makes to distillate at the top of container by the steam G2 of piping t8 supply, by matching Pipe t9 is supplied to the 1st gas-liquid separation container 11 as steam G3.

Also, the height of the liquid level of the concentrate to the bottom for being maintained at container is provided in the 2nd gas-liquid separation container 21 Spend the liquidometer S2 measured the and thermometer T2 measured to the temperature of concentrate.

It should be noted that the 2nd gas-liquid separation container 21 and the 1st gas-liquid separation container 11 are same, it is not limited to the structure of Fig. 1 At.

In addition, in Fig. 1 although not shown, but in the 2nd gas-liquid separation container 21, can container inside and than piping t8 Junction it is top position setting as in the 1st gas-liquid separation container 11 setting as gas-liquid separator 13.

(the 2nd evaporator)

2nd evaporator 22 will go out tank from the 2nd gas-liquid separation container 21 and be heated simultaneously by the concentrate that piping t6, t7 are supplied Evaporation.Then, generated steam G2 is supplied to the 2nd gas-liquid separation container 21 by being piped t8 by the 2nd evaporator 22.

It should be noted that the 2nd evaporator 22 and the 1st evaporator 12 it is also possible to using various compositions equipment.

(connecing liquid position: position)

2nd evaporator 22 (the 2nd gas-liquid separation unit 20) as the position for heating concentrate and contacted with concentrate Connect liquid position to fixedness ingredient in resistance to adhesion.

Being somebody's turn to do " connecing liquid position " for example is to generate transfer of the thermal energy from thermal medium H to concentrate in the 2nd evaporator 22 Position, and be in the wall surface for the component (pipe, plate etc.) of concentrate being spaced apart, concentrate side by thermal medium H (with concentrate The side of contact) face.

(connecing liquid position: state)

Should " being in resistance to adhesion to fixedness ingredient " refer to implement present fixedness ingredient be precipitated be difficult to it is attached State processing, in particular to " state being coated by the material of resistance to adhesion " or " flat state ".

" by the material of resistance to adhesion be coated state " refer to, the material of resistance to adhesion relative to connect liquid position with 1~100 μm, The coating state of preferably 5~50 μm of thickness.By make the material of resistance to adhesion with a thickness of specified value more than, can make resistance to attached Property it is reliable, and by make the material of resistance to adhesion with a thickness of specified value hereinafter, the reduction of heat transfer efficiency can be inhibited.

Also, for the material of resistance to adhesion, such as organic based material, can enumerate (methyl) acrylic resin, Epoxy resin, polyurethane resin, organic siliconresin, fluororesin, polyimide resin, polyether-ether-ketone resin, polyolefin resin Deng, as inorganic based material, the containing metal oxide coating in resistance to adhesion can be enumerated, contain carbon coating etc., but do not limit In these.

In the case that the liquid to be treated for containing photoresist (resin) especially stated afterwards is as object, resistance to attachment Property material be preferably fluororesin, polyether-ether-ketone resin, containing metal oxide coating and at least one of containing carbon coating.

It should be noted that as fluororesin, it is specific enumerable go out: polytetrafluoroethylene (PTFE), perfluoroalkoxyalkane, tetrafluoro second Alkene-ethylene copolymer, tetrafluoraoethylene-hexafluoropropylene copolymer etc..

" flat state " refers to that surface roughness is 1 μm of state below.Also, the method for forming " flat state " It can be and implement electrolytic polishing, the milled processeds such as polishing grinding by the liquid position that connects to the 2nd evaporator 22 and make rough surface Degree is specified value the following method, is also possible to select surface roughness as specified value material below (plate etc.) and be applied to The method for connecing liquid position of 2nd evaporator 22.

It should be noted that the surface roughness specifically refers to arithmetic average roughness (Ra).

(solid removal unit)

Solid removal unit 40 is the solid (fixedness ingredient being precipitated etc.) that will contain in concentrate from concentrate The unit of middle removal.The solid removal unit 40 plays the effect for preventing solid from flowing into aftermentioned pump.

As long as the equipment that solid removal unit 40 can separate solid from liquid is not particularly limited, example Bucket type filter, filter, liquid cyclones, centrifugal sedimentation device, standing sedimentation device can such as be applied.

It should be noted that solid removal unit 40 is can be set in fixedness in Fig. 1 at analyzing possibility height The 2nd gas-liquid separation container 21 and the 2nd evaporator 22 between, also can be set in the 1st gas-liquid separation container 11 and the 1st evaporator Between 12.

<pump>

Pump P1 conveys concentrate from the 1st gas-liquid separation container 11 to the 1st evaporator 12 by being piped t2, t3, and passes through Piping t2, t5 convey concentrate from the 1st gas-liquid separation container 11 to the 2nd gas-liquid separation container 21.

Pump P2 conveys concentrate from the 2nd gas-liquid separation container 21 to the 2nd evaporator 22 by being piped t6, t7, and passes through It is piped t6, t11 and conveys concentrate from the 2nd gas-liquid separation container 21 to outside.

As long as can be applied well known it should be noted that pump is not particularly limited for that can convey the composition of liquid Pump.As long as in addition, pump setting position can between each component in suitably convey concentrate, be not limited to the setting of Fig. 1 Position can also suitably increase and decrease the setting quantity of pump.

<valve>

Valve V1 is adjusted to by piping t1 externally to the flow for the liquid to be treated L1 that the 1st gas-liquid separation container 11 supplies Section.

Valve V2 is to the flow by being piped the concentrate that t2, t3 are supplied from the 1st gas-liquid separation container 11 to the 1st evaporator 12 It is adjusted.

Valve V3 is to the concentrate supplied by being piped t2, t5 from the 1st gas-liquid separation container 11 to the 2nd gas-liquid separation container 21 Flow be adjusted.

Valve V4 is to the flow by being piped the concentrate that t6, t7 are supplied from the 2nd gas-liquid separation container 21 to the 2nd evaporator 22 It is adjusted.

Valve V5 is adjusted to by piping t6, t11 from the 2nd gas-liquid separation container 21 to the flow of the concentrate of outside discharge Section.

It should be noted that as long as valve is that can be adjusted by adjusting of level (degree of flow path ON/OFF) of switch etc. The composition for saving the flow of liquid is not particularly limited, and can apply well known valve.In addition, as long as the setting position of valve can be The flow that concentrate is suitably adjusted between each component is then not limited to the setting position of Fig. 1, can also appropriate regulating valve set Set quantity.

<metrical instrument>

Function Solution Handling Device Used 1A is also equipped with other than liquidometer S1, S2 above-mentioned, thermometer T1, T2 in each piping Solution (liquid to be treated, concentrate) flow flowmeter F1, F2, F3, F4 for being measured.

As long as these metrical instruments are that can obtain the composition of desired information to be not particularly limited, can be using public affairs The metrical instrument known.

<control unit>

Control unit 30 is to read data and according to the data from each metrical instrument come the unit of control valve etc..Moreover, control Unit 30 processed has storage unit (not shown) of the storage as the data of the benchmark of control.

It should be noted that being discussed in detail below using the control method of control unit 30.

The operation that control unit 30 passes through the program based on CPU (Central Processing Unit, central processing unit) Processing, special circuit etc. are realized.In addition, the storage unit that control unit 30 has can be by RAM (Random Access Memory, random access memory), ROM (Read Only Memory, read-only memory), HDD (Hard Disk Drive, Hard disk drive), the conventional memory devices such as flash memory constitute.

Then, the liquid to be treated of the process object of the Function Solution Handling Device Used as present embodiment is illustrated.

" liquid to be treated "

Liquid to be treated L1 is the solution containing organic solvent and fixedness ingredient.

Also, for liquid to be treated L1, such as the photoetching work when manufacturing crystal liquid substrate, semiconductor integrated circuit can be enumerated The stripper containing the resin (fixedness ingredient) for being referred to as photoresist generated in sequence.

It as the organic solvent of liquid to be treated L1, such as can enumerate: monoethanolamine, dimethyl sulfoxide, diethylene glycol list Butyl ether, glycol monoethyl ether, propylene glycol methyl ether acetate, propylene glycol monomethyl ether etc., but not limited to this.

As the fixedness ingredient of liquid to be treated L1, such as the resins (photonasty such as can enumerate photoresist above-mentioned Resin material), specifically it is assumed that novolac resin, but it is not limited to these.

It should be noted that is contained in liquid to be treated L1 is non-volatile from the perspective of properly implementing separating treatment The content of property ingredient (resin) is preferably 0.1~5.0 mass %.

Then, " the fixedness ingredient " of liquid to be treated L1 refers to nonvolatile ingredient in Function Solution Handling Device Used operation, Refer to the boiling point under the pressure in evaporator (the 1st evaporator 12 and the 2nd evaporator 22) operation of Function Solution Handling Device Used in detail The ingredient higher than the heating temperature of the evaporator.Therefore, it as fixedness ingredient, other than aforementioned resin, can also enumerate Out: crystal liquid substrate, semiconductor integrated circuit manufacture when the suspended materials such as the particles of inorganic material that generates, be also dissolved in and located Manage the higher boiling ingredient (such as the ingredients such as sorbierite contained in anticorrosive, preservative) of liquid L1.

It should be noted that the whole contained in liquid to be treated L1 is not from the perspective of properly implementing separating treatment The content (total amount) of volatile component is more preferably 0.1~5.0 mass %.

Not only contain in the case that resin also contains suspended material as fixedness ingredient in liquid to be treated L1, institute The resin of precipitation agglomerates suspended material, as a result exist make the 2nd evaporator 22 it is equal in be precipitated substance (properly termed as " and be precipitated at Point ") size, amount increase tendency.Even however, in this case, according to the present invention, being also able to suppress precipitation ingredient In the attachment for connecing liquid position of the 2nd evaporator 22, properly concentrate is heated and obtains (the excellent processing of desired effect Efficiency).

It should be noted that can be with other than organic solvent above-mentioned, fixedness ingredient in liquid to be treated L1 Contain water.

Then, the solution processing methods of present embodiment are illustrated referring to Fig.1.It should be noted that aforementioned reality The movement for applying the Function Solution Handling Device Used of mode is also illustrated together.

" solution processing methods of present embodiment "

The solution processing methods of present embodiment include the 1st gas-liquid separation process and the 2nd gas-liquid separation process.

Hereinafter, being illustrated to each process.

<the 1st gas-liquid separation process>

1st gas-liquid separation process refers to liquid to be treated L1 heating, distillates steam and make kept concentrate The process that a part goes out tank.

Specifically, the 1st gas-liquid separation process will go out tank from the 1st gas-liquid separation container 11 using the 1st evaporator 12 and lead to The concentrate for crossing piping t2, t3 supply is heated and is evaporated.Then, by the steam G1 generated in the 1st evaporator 12 and heated Concentrate by be piped t4 be supplied to the 1st gas-liquid separation container 11.Then, make the gas-liquid using the 1st gas-liquid separation container 11 Separator 13 distillate at the top of the vapors from vessel of gas-liquid separation, is passed out to as steam G4 is distillated by being piped t10 It is external.On the other hand, by the concentrate flowed down by the condensation of the gas-liquid separator 13 of the 1st gas-liquid separation container 11 in container Bottom keeps specified amount, and it is made to go out tank from bottom with defined flow.Then, which is supplied to the 1st Evaporator 12 and the 2nd gas-liquid separation container 21.

Also, in the 1st gas-liquid separation process, the 1st gas-liquid separation unit 10 is controlled so as to contain not in liquid to be treated Volatile component is not precipitated.

The content of the control in specific 1st gas-liquid separation process is illustrated below, but is not limited to the following contents.

Firstly, the liquid to be treated L1 used as object is real in advance under conditions of simulating the condition in physical device Evaporation and concentration test is applied, what inspection fixedness ingredient started to be precipitated distillates rate (properly termed as " the 1st distillates rate ") and concentrate Temperature (properly termed as " the 1st concentrate temperature "), gained the 1st is distillated into rate and the 1st concentrate temperature is stored in control unit 30 storage unit.

It should be noted that the rate that distillates that fixedness ingredient is precipitated in prior evaporation and concentration test is 83% In the case where, the value (for example, 80%) more smaller than the numerical value can be set as " the 1st distillates rate ", in fixedness at distribution In the case that the raw concentrate temperature being precipitated is 97.7 DEG C, the value (for example, 97 DEG C) more smaller than the numerical value can be set as " the 1st concentrate temperature ".

In 1st gas-liquid separation process, control unit 30 reads the data on flows of the liquid to be treated L1 of flowmeter F1, flowmeter The data on flows of the concentrate of F2.Then, control unit 30 calculates distillating for the 1st gas-liquid separation unit 10 according to these data Rate the 1st distillates rate and is compared be stored in storage unit.In the case where the rate that distillates distillates rate or more for the 1st, control unit In the control of the level (degree that flow path is opened) of the aperture of 30 implementation increase valve V1, the horizontal control of the aperture of increase valve V3 At least one kind of control.On the other hand, calculated distillate rate it is too low in the case where, control unit 30 implement with aforementioned control Opposite control.

In addition, control unit 30 reads the temperature data of thermometer T1 in the 1st gas-liquid separation process.Then, control unit 30 are compared the temperature of read concentrate with the 1st concentrate temperature for being stored in storage unit.In the temperature of concentrate In the case where more than 1st concentrate temperature, the heating temperature that control unit 30 implements to reduce the 1st evaporator 12 (reduces heat to be situated between The temperature of matter H, the flow for reducing thermal medium H) control, increase valve V1 aperture horizontal control, increase the aperture of valve V3 Horizontal control at least one kind of control.On the other hand, in the case where the temperature of concentrate is too low, control unit 30 is real Grant the opposite control of aforementioned control.

It should be noted that suitable at the time of control (reading of data is compared, the control of valve etc.) based on control unit 30 When using specified interval or the continuously setting implemented, in turn, can be increase after reaching steady state the moment interval (or Stop control) setting.It is also the same in control below about the point.

In the 1st gas-liquid separation process, from make the maintenance dose of the concentrate in the 1st gas-liquid separation container 11 in prescribed limit From the perspective of interior, it is possible to implement control as follows.

In 1st gas-liquid separation process, control unit 30 reads the fluid level data of liquidometer S1.Then, control unit 30 Calculate the amount of concentrate that the 1st gas-liquid separation container 11 is kept according to the data, and be stored in storage unit defined amount (on Limitation, lower limit amount) compare.In the case where the amount of the concentrate calculated reaches upper limit amount, control unit 30 is implemented to increase valve At least one kind of control in the horizontal control of the aperture of V3, the horizontal control for the aperture for reducing valve V1.In addition, being calculated Concentrate amount reach lower limit amount in the case where, implement the control opposite with aforementioned control.

Aforementioned " distillating rate " in 1st gas-liquid separation process refers to, for example, in liquid to be treated L1 with 1000kg/h to the 1st gas It, can in the case that the supply of liquid separation vessel 11, concentrate are supplied with 200kg/h to the 2nd gas-liquid separation container 21 by piping t5 To calculate as 80% (=(1000-200)/1000 × 100).That is, the 1st gas-liquid separation process (the 1st gas-liquid separation unit 10) The rate of distillating can be calculated according to the data on flows of flowmeter F1 and flowmeter F2.

In addition, the state of aforementioned " precipitation of fixedness ingredient " refers to, because heating liquid to be treated L1 due to not waving for being precipitated Hair property ingredient is attached to the state of the wall surface of evaporator, piping etc..In other words refer to, since fixedness is at analyzing and adhere to In evaporator (the 1st evaporator 12 is concentrated by evaporation evaporator used in test), lead to evaporator of the overall heat-transfer coefficient from script (unattached fixedness ingredient, heat transfer efficiency do not have total biography of the evaporator of reduced state to shown overall heat-transfer coefficient completely Hot coefficient) reduce by 10% or more state.It should be noted that the overall heat-transfer coefficient of the coefficient of the performance as display evaporator U can be very according to " Q (exchange heat: kcal/hr)=U (overall heat-transfer coefficient: kcal/m²Hr DEG C) × A (heat transfer area: m²)×ΔT The formula of (average temperature difference of heated medium and thermal medium: DEG C) " calculates.

<the 2nd gas-liquid separation process>

2nd gas-liquid separation process refers to, by the concentrate heating for going out tank in the 1st gas-liquid separation process, distillates steam simultaneously And a part of kept concentrate is made to go out the process of tank.

Specifically, the 2nd gas-liquid separation process will go out tank from the 2nd gas-liquid separation container 21 using the 2nd evaporator 22 and lead to The concentrate for crossing piping t6, t7 supply is heated and is evaporated.Then, the steam G2 generated in the 2nd evaporator 22 is passed through into piping T8 is supplied to the 2nd gas-liquid separation container 21.Then, the steam is evaporated as steam G3 from the top of the 2nd gas-liquid separation container 21 Out, the 1st gas-liquid separation container 11 is supplied to by being piped t9.

Also, in the 2nd gas-liquid separation process, it is controlled such that the temperature of kept concentrate is the upper of the rate that distillates Rise the predetermined temperature stagnated or less.

The content of the control in specific 2nd gas-liquid separation process is illustrated below, but is not limited in below Hold.

Firstly, the liquid to be treated L1 used as object is real in advance under conditions of simulating the condition in physical device Evaporation and concentration test is applied, inspection distillates the temperature (properly termed as " limit concentrate temperature ") that the rising of rate is stagnated, by institute Obtain the storage unit that limit concentrate temperature is stored in control unit 30.

It should be noted that the temperature that the rising for distillating rate in prior evaporation and concentration test is stagnated is 99.4 DEG C In the case where, the value (for example, 99 DEG C) more smaller than the numerical value can be set as " limit concentrate temperature ".

In 2nd gas-liquid separation process, control unit 30 reads the temperature data of thermometer T2.Then, control unit 30 will The temperature of read concentrate is compared with the limit concentrate temperature for being stored in storage unit.It oversteps the extreme limit in the temperature of concentrate In the case where concentrate temperature, control unit 30 implements to increase the horizontal control of the aperture of valve V5, the aperture for increasing valve V3 The control of the heating temperature (reduce the temperature of thermal medium H, reduce the flow of thermal medium H) of horizontal control, the 2nd evaporator 22 of reduction At least one kind of control in system.It should be noted that control unit 30 is implemented with before in the case where the temperature of concentrate is too low It states and controls opposite control.

In the 2nd gas-liquid separation process, from piping t11 concentrate L2 is discharged to the outside when, can be it is aforementioned this The scheme of specified amount is always discharged under kind control, is also possible to the scheme being discharged as follows at the regulation moment.

Specifically, control unit 30 reads the fluid level data of liquidometer S2 in the 2nd gas-liquid separation process.Then, it controls Unit 30 processed calculates the amount of concentrate that the 2nd gas-liquid separation container 21 is kept according to the data, and be stored in storage unit Defined amount (upper limit amount, lower limit amount) is compared.It can be following scheme: reaching upper limit amount in the amount of the concentrate calculated At the time of, implementation makes valve V5 from the control closed → opened, and at the time of reaching lower limit amount, implementation makes valve V5 from the control opened → closed.

In addition, control unit 30 reads the temperature data of thermometer T2 in the 2nd gas-liquid separation process.Then, control is single The temperature of read concentrate is compared by member 30 with the limit concentrate temperature for being stored in storage unit.In the temperature of concentrate Degree reach capacity concentrate temperature at the time of, implementation make valve V5 from the control closed → opened.It should be noted that make valve V5 from open → As previously mentioned, at the time of reaching lower limit amount using the amount of the concentrate calculated according to the fluid level data of liquidometer S2 i.e. at the time of pass It can.

(flow velocity of the concentrate in the 2nd gas-liquid separation process)

In the 2nd gas-liquid separation process, the flow control of the concentrate in the 2nd evaporator 22 is not made to be precipitated not The flow velocity of volatile component accumulation, specially 0.5~2.0m/s, preferably 1m/s or more.

It is more than the speed specified value by making the concentrate in the 2nd evaporator 22, though fixedness at analyzing, It can inhibit the accumulation that ingredient is precipitated in the 2nd evaporator 2, therefore ingredient can be precipitated with very high horizontal inhibition and connect liquid The attachment at position.

Specifically, implementing control as follows.

In 2nd gas-liquid separation process, control unit 30 reads the data on flows of flowmeter F3.Then, control unit 30 will The flow velocity of the concentrate in the 2nd evaporator 22 calculated according to read data on flows and the regulation flow velocity for being stored in storage unit (such as 0.5m/s above-mentioned) compares.In the case where the flow velocity of concentrate is less than regulation flow velocity, control unit 30 implements enhancing Pump the horizontal control of the conveying of P2.On the other hand, in the case where the flow velocity of concentrate is excessive, control unit 30 is implemented with before It states and controls opposite control.

It should be noted that the flow velocity of the concentrate in the 2nd evaporator 22 can according to the data on flows of flowmeter F3 and The area of section for the logical circulation road that the concentrate of 2nd evaporator 22 is flowed through calculates.Such as the 2nd evaporator 22 be multitube heat hand over In the case that parallel operation and concentrate flow through in multiple pipes, by the way that the area of section adduction of the inside of each pipe is calculated total cross section face Product, and by the value (m of data on flows³/ s) divided by the total cross-sectional area (m²), the flow velocity (m/s) of concentrate can be calculated.

(flow velocity of the concentrate in the 2nd gas-liquid separation process: the judgement of the calculating formula based on sinking speed)

When fluid is laminar flow, in the density for setting particle as ρ_p(kg/m³), the density of fluid be ρ_f(kg/m³), generation of particle Table diameter is d_p(m), acceleration of gravity is g (m/s²), fluid viscosity be η (Pas) in the case where, the sinking speed V of particle (m/s) " V=(ρ can be used_p-ρ_f)d_p ²G/ (18 η) " is indicated.

The formula is well known formula as the formula for calculating sinking speed, is suitable for the case where Reynolds number is less than 6 Formula, the diameter for being particularly well suited to the particle as object is the situation of 1mm or less.

For example it is assumed that removing that diameter is more than 1mm with filter in order to avoid these troubles of the blocking in piping etc. Grain, in the case where the representative diameter of particle is defined as 1mm, the density of fluid uses 1000kg/m³, particle density use 2000kg/m³, fluid viscosity use 0.01Pas when, the sinking speed of the particle can calculate about 0.05m/s.It needs Illustrate, Reynolds number in this case is 5.45, less than 6.

Accordingly, it is considered to when sinking speed (the about 0.05m/s) of particle into fluid, it is known that by making concentrate with the speed 10 times of flow velocity (0.5m/s or more) flowing of degree, before the accumulation so as to prevent the precipitation ingredient in the 2nd evaporator 22 It is safe for stating judgement.

" function and effect "

According to the Function Solution Handling Device Used and solution processing methods of the above this present embodiment, following effect can be played Effect.

The Function Solution Handling Device Used and solution processing methods of present embodiment utilize so that is contained in liquid to be treated is non-volatile The 1st gas-liquid separation unit (the 1st gas-liquid separation process) and connect liquid position to not that the mode that property ingredient is not precipitated is controlled Volatile component implements gas-liquid separation processing in the 2nd gas-liquid separation unit (the 2nd gas-liquid separation process) of resistance to adhesion.That is, The Function Solution Handling Device Used and solution processing methods of present embodiment not only implement 2 grades of gas-liquid separation processing, but also in the 2nd gas-liquid Separative unit (the 2nd gas-liquid separation process) though in the fixedness of liquid to be treated at branch be precipitated it is high-caliber under the conditions of Implement evaporation process, the reduction with the treatment effeciency that ingredient attachment is precipitated can also be inhibited.Therefore, according to the present embodiment Function Solution Handling Device Used and solution processing methods, even if the fixedness of liquid to be treated at analyzing, can also play excellent place Manage efficiency.

" variation "

More than, the Function Solution Handling Device Used and solution processing methods of present embodiment are illustrated, but present embodiment It is not limited to this, such as can be changed as follows.

The Function Solution Handling Device Used 1A of Fig. 1 makes the 1st gas-liquid separation container 11 and the 1st evaporator 12 is respectively individual device, But Function Solution Handling Device Used 1B that can also be as shown in Figure 2 is such, by being arranged the 1st evaporator 102 in the 1st gas-liquid separation container Make the 1st gas-liquid separation unit 100 integrated in 101.

It should be noted that the composition of the 1st gas-liquid separation unit 100 shown in Fig. 2 are as follows: in order to will remain in the 1st The concentrate of the bottom of gas-liquid separation container 101 heats and has (the 1st evaporation of heat-transfer pipe 102 for having thermal medium H in internal circulation Device 102).

As previously mentioned, as long as the equipment that concentrate can be heated and be evaporated by the 2nd evaporator 22 is not particularly limited, It can be heat-exchangers of the plate type 202 as shown in Figure 2 (the 2nd evaporator 202).

In the 2nd gas-liquid separation unit 20 shown in Fig. 1, since the concentration of fixedness ingredient increases, concentrate becomes A possibility that being easy cured state (or viscosity high and be difficult to the state flowed) is high.Therefore, it can be set the 2nd gas-liquid separation Concentrate in unit 20 is heated up to the heating unit of not cured horizontal (or level of the viscosity of available pump P2 conveying).

It should be noted that as long as heating unit is from the position circulated to concentrate, (specially the 2nd gas-liquid separation is held The bottom of the holding concentrate of device 21 and piping t6, t7, t11) it is not particularly limited from the external equipment for applying heat, it can enumerate Heating position can be impregnated in the hot solvent storage tank of thermal medium, heater etc. out.

The liquid position that connects contacted with concentrate to the 2nd evaporator 22 shown in FIG. 1 is in resistance to attachment to fixedness ingredient Property the case where be illustrated, but be not limited to this in the position of resistance to adhesion and connect liquid position.

For example, following scheme can be used: for the position circulated as the concentrate in the 2nd gas-liquid separation unit 20 (bottom of the holding concentrate of specially the 2nd gas-liquid separation container 21 and piping t6, t7, t11) and in being contacted with concentrate Side is also in resistance to adhesion.

It should be noted that can using the scheme for connecing liquid position also and be in resistance to adhesion in the 1st evaporator 12, it is contemplated that The expense of processing can be generated, and the conductivity of heat in the 1st evaporator 12 reduces, treatment effeciency on the whole slightly reduces.

To the amount for the concentrate that the 2nd gas-liquid separation container 21 according to figure 1 is kept come the scheme of control valve V5 into Gone explanation but it is also possible to be the pace of change (speed that liquid level rises) according to the liquid level of concentrate come the scheme of control valve 5.

Such as it can be following scheme: the fluid level data of the reading of control unit 30 liquidometer S2.Then, control unit 30 will According to the pace of change of the liquid level of the concentrate in the 2nd evaporator 22 of read fluid level data calculating and it is stored in storage unit Defined speed be compared.At the time of the pace of change of the liquid level of concentrate is less than defined speed, implementation makes valve V5 From the control closed → opened.

The fixedness ingredient (photoresist) contained in liquid to be treated L1 is the ingredient containing sulphur atom, for example wraps In the case where containing resist of 1,2- naphthalene quinone di-azide sulfonic acid ester (NQD) class compound as photosensitizer etc., can using " fixedness component amount ", the scheme of " viscosity " are measured in 2nd gas-liquid separation container 21 as shown below.

The measurement of the NQD class compound (fixedness ingredient) contained in the concentrate of 2nd gas-liquid separation container 21 can be with According to using the obtained data of fluorescent X-ray sulphur content analysis apparatus to calculate.Here, the photograph for passing through fluorescent X-ray due to sulphur atom The fluorescent X-ray of the energy of about 2.3keV is penetrated and issues, therefore by measuring the amount of x-ray generated by sulphur atom from spectrum, It can carry out the quantitative analysis of sulphur concentration.Then, bent according to the result of the quantitative analysis of sulphur concentration and pre-rendered good standard Line can calculate " fixedness component amount ", " viscosity " in the concentrate of the 2nd gas-liquid separation container 21.

It should be noted that in the case where carrying out this measurement following scheme can be used: by the 2nd gas-liquid point The piping that a part of concentrate is extracted out/sent back to is arranged in lower part from container 21, and be arranged in the piping T junction and Valve connects the piping supplied to fluorescent X-ray sulphur content analysis apparatus on the T word connector, can carry out METHOD FOR CONTINUOUS DETERMINATION.

Furthermore, it is possible to using " fixedness obtained from being measured according to the concentrate to the 2nd gas-liquid separation container 21 Component amount ", " viscosity " carry out the scheme of control valve V5, and (at the time of fixedness component amount reaches specified amount or more or viscosity reaches Make valve V5 from closing → open at the time of more than to specified value).