阅读说明：本技术 一种用于木糖制备中离子交换柱的复苏方法及系统 (Recovery method and system for ion exchange column in xylose preparation ) 是由 吴限智 陈德水 徐小荣 莫世清 黄钱威 于 2019-08-06 设计创作，主要内容包括：本发明公开一种用于木糖制备中离子交换柱的复苏方法及系统,属于离子交换柱复再生技术领域。复苏方法结合复苏系统,以流速为5～10m/h,向待复苏的离子交换柱中注入复苏剂,在温度为40～45℃的条件下复苏24h以上；所述复苏剂以质量百分比计,包括如下组分：漂白粉0.1～0.15%、双氧水1～1.5%、氯化钠7～8%及氢氧化钠2～2.5%。解决采用已有技术中,木糖溶液中杂质被离子交换树脂吸附而不能被常规的解吸附剂解析,而长期滞留于树脂中,从而导致树脂被污染等问问题,本发明实现复苏后树脂交换倍数提高至接近原有水平,并延长其使用寿命,同时,有效节约水资源,并减少再生排放废液中的含糖量和COD。(The invention discloses a recovery method and a recovery system for an ion exchange column in xylose preparation, and belongs to the technical field of ion exchange column regeneration. The recovery method is combined with a recovery system, a recovery agent is injected into an ion exchange column to be recovered at the flow rate of 5-10 m/h, and recovery is carried out for more than 24h at the temperature of 40-45 ℃; the resuscitation agent comprises the following components in percentage by mass: 0.1-0.15% of bleaching powder, 1-1.5% of hydrogen peroxide, 7-8% of sodium chloride and 2-2.5% of sodium hydroxide. The method solves the problems that impurities in the xylose solution are adsorbed by ion exchange resin and can not be resolved by conventional desorbent, and are retained in the resin for a long time, so that the resin is polluted and the like in the prior art.)

1. a recovery method of an ion exchange column used in xylose preparation is characterized in that: the method comprises the steps of injecting a resuscitation agent into an ion exchange column to be resuscitated at a flow rate of 5-10 m/h, and resuscitating for more than 24h at a temperature of 40-45 ℃ to obtain the resuscitated ion exchange column.

2. The method for the resuscitation of ion exchange columns used in the preparation of xylose according to claim 1, characterized in that: the ion exchange column to be recovered is an ion exchange column of which the ion exchange multiple is reduced to 75-85% of the original exchange multiple, and the exchange capacity is reduced by 20-30% compared with the normal operation of the ion exchange column after regeneration.

3. The method for the resuscitation of ion exchange columns used in the preparation of xylose according to claim 1, characterized in that: the resuscitation agent comprises the following components in percentage by mass: 0.1-0.15% of bleaching powder, 1-1.5% of hydrogen peroxide, 7-8% of sodium chloride and 2-2.5% of sodium hydroxide.

4. The method for the resuscitation of ion exchange columns used in the preparation of xylose according to claim 1 or 3, characterized in that: the content of available chlorine in the bleaching powder is 30-38%.

5. The method for the resuscitation of ion exchange columns used in the preparation of xylose according to claim 1, characterized in that: the preparation method of the resuscitation agent comprises the steps of sequentially adding bleaching powder, hydrogen peroxide, sodium chloride and sodium hydroxide into a preparation tank, and stirring for more than 1h for later use; after the resuscitation agent is prepared, the standing time cannot exceed 12 h.

6. The method for the resuscitation of ion exchange columns used in the preparation of xylose according to claim 1, characterized in that: before the injection of the resuscitation agent, pretreating the ion exchange column to be resuscitated, wherein the pretreatment comprises small backwashing, specifically, opening a liquid discharge valve (112) in the middle of the ion exchange column (1), introducing cleaning water into the ion exchange column (1) through an intermediate liquid discharge device, and carrying out the small backwashing for 5min at the flow speed of 10 m/h; and finally, opening a water inlet valve (110) at the upper part of the ion exchange column (1) and discharging accumulated water in the ion exchange column (1) to the surface of the fat pressing layer (121).

7. the method for the resuscitation of ion exchange columns used in the preparation of xylose according to claim 1 or 6, characterized in that: after the ion exchange column is revived, carrying out post-treatment on the ion exchange column, wherein the post-treatment comprises small forward washing, and specifically, opening a water inlet valve (110) at the upper part of the ion exchange column (1), introducing cleaning water into the ion exchange column (1), and carrying out the small forward washing at the flow speed of 20-30 m/h; and finally, opening a liquid discharge valve (112) in the middle of the ion exchange column (1) until the refraction of the solution in the liquid discharge valve (112) is less than 1.

8. The method for the resuscitation of ion exchange columns used in the preparation of xylose according to claim 1, characterized in that: and detecting the recovered ion exchange column to obtain that the resin exchange amount is increased by 30-50%, the water consumption is reduced by 30-40%, the discharging refraction is 7-8, the conductivity is lower than 500us/cm, and the light transmittance is higher than 90.

9. A resuscitation system for use with an ion exchange column in xylose production according to claim 1, wherein: the device comprises an ion exchange column (1), a cleaning water storage tank (2) and a resuscitation agent storage tank (3), wherein the cleaning water storage tank (2) is connected with the ion exchange column (1) through a conveying pipe I (4), and the resuscitation agent storage tank (3) is connected with the ion exchange column (1) through a conveying pipe II (5); and control valves (6) are arranged on the conveying pipe I (4) and the conveying pipe II (5).

10. The resuscitation system for use with an ion exchange column for xylose production according to claim 9, wherein: the ion exchange column (1) comprises a tank body (11) and a cavity (12) arranged in the tank body (11), wherein a water inlet valve (110) and a resuscitation agent inlet valve (111) are arranged at the upper part of the tank body (11), and a liquid discharge valve (112) is arranged in the middle of the tank body (11); resin (120) is arranged in the cavity (12), and a grease pressing layer (121) is arranged on the surface layer of the resin (120); the middle part of the cavity (12) is provided with an intermediate liquid drainage device which forms a passage with a liquid drainage valve (112);

The upper portion of the tank body (11) is further provided with a feeding hole (113) and a radar liquid level meter hole (114), the bottom end of the tank body is provided with a discharging hole (115), a feeding distributor (122) is arranged in the tank body (11), and the feeding distributor (122) and the feeding hole (113) form a passage.

Technical Field

The invention relates to a recovery method and a recovery system for an ion exchange column, in particular to a recovery method and a recovery system for an ion exchange column in xylose preparation, and belongs to the technical field of ion exchange column regeneration.

Background

In the process of preparing xylose by using hemicellulose as a raw material, the process specifically comprises the following steps: under the heating condition, sulfuric acid is added into raw material hemicellulose, the hemicellulose is hydrolyzed into xylose and other miscellaneous sugars by the sulfuric acid, meanwhile, impurities such as sulfate ions, organic acid radical ions (mainly phenolic substances) and sodium ions exist in a hydrolysis liquid, and the generated xylose exists in a solution state, so in order to improve the quality of the xylose, the impurities such as the sulfate ions, the organic acid radical ions (mainly phenolic substances), the sodium ions, the calcium ions and the magnesium ions in the hemicellulose hydrolysis liquid need to be effectively removed.

the ion exchange column is a column-shaped pressure vessel for performing an ion exchange reaction, and is an exchange apparatus for ion exchange by a column method. The xylose solution containing impurities is introduced from one end of the column and is in full contact with the fixed ion exchange resin layer in a dense state or the ion exchange resin bed in a flowing state in the column, so that ion exchange is carried out, finally, the pure xylose solution flows out from the other end of the column, and the impurities in the xylose solution are combined on the resin. However, with the progress of the purification process, the resin in the ion exchange column is finally in a "saturated state", the adsorption capacity of the resin to impurity ions in the xylose solution is gradually reduced, and the problems of low adsorption strength, small exchange amount and the like occur, the column exchange needs to be cut off from the production line, the ion exchange column in the "saturated state" is replaced, desorption liquid is desorbed for the replaced ion exchange column, the regeneration of the ion exchange column is realized, and the cyclic utilization of the ion exchange column is realized.

On 2010, 09/22, a patent document with publication number CN101837305A entitled "a method and apparatus for regenerating ion exchange resin" is disclosed, which specifically discloses: dividing the acid or alkali liquor with the amount required by the regenerated ion exchange resin into three times of entering and exiting the ion exchange column, and recovering the acid or alkali liquor discharged at the last time. The invention also relates to a device for implementing the method. The device includes: acid-base device, first pipeline, first valve, acid-base recovery unit, second pipeline, second valve, third pipeline, third valve. The acid-base device is connected with the first pipeline, the first pipeline is used for being connected with an ion exchange column, the ion exchange column is connected with the second pipeline, and the second pipeline is connected with the third pipeline and the acid-base recovery device. The first valve, the second valve and the third valve are respectively arranged on the first pipeline, the second pipeline and the third pipeline. The invention solves the problems that the prior regeneration method of the ion exchange resin generates a large amount of waste liquid and the waste liquid can not be recycled.

A patent document having publication No. CN101224436A entitled "a method for regenerating ion exchange resin" was disclosed at 23.07.2008, in which: the ion exchange resin includes cation exchange resin and anion exchange resin, and the method includes mainly the steps of introducing the solution into ion exchange column with ion exchange resin to eliminate impurity ion adsorbed or firmly combined to the resin and introducing the regenerated liquid into the ion exchange column to restore the ion exchange capacity of the ion exchange resin. The desorption solution and the regeneration solution are respectively introduced into the ion exchange column in a forward flow mode and a reverse flow mode. When the cation exchange resin is H⁺When the cation exchange resin is used for the cation exchange resin, the analytic solution is a sodium hydroxide solution, and the regenerated solution is an inorganic acid solution; when the anion exchange resin is OH^-When the anion exchange resin is formed, the analytic solution is hydrochloric acid solution, and the regeneration solution is sodium hydroxide or potassium hydroxide solution.

A patent document having publication No. CN105562126A entitled "a method for regenerating an anion exchange resin" was disclosed at 11/05/2016, and specifically disclosed therein: the regeneration method of the anion exchange resin is characterized by comprising the steps of filling a wet method into a column at the temperature of 5-50 ℃, filling the anion exchange resin to be regenerated into a glass chromatographic column, wherein the diameter-height ratio is 1: 2-1: 8, passing 0.5-8 BV of an alcohol-base solution through the anion exchange column, washing with water until the PH is less than or equal to 9, passing 0.5-6 BV of a hydrochloric acid solution through the anion exchange column, washing with water until the PH is greater than or equal to 5, and finally introducing 0.5-6 BV of a sodium hydroxide solution into the anion exchange column, washing with water until the PH is less than or equal to 9, namely completing the regeneration of the anion exchange resin. The invention overcomes the defects of the prior method for regenerating the anion exchange resin in the stevioside production, greatly improves the regeneration exchange capacity of the anion exchange resin, obviously increases the treatment capacity and prolongs the regeneration period.

In the prior art, for resin regeneration in an ion exchange column, water, alkali, acid, alcohol-alkali solution or diethyltoluene and the like are generally adopted for treatment, but the method has poor practicability and certain limitations when aiming at different working conditions, such as: in the practical application of the process for preparing xylose by hydrolyzing hemicellulose, after an ion exchange column is in a saturated state, water is used for flushing out residual materials, which cannot be completely flushed; moreover, when the alkali liquor is added for regeneration, the residual xylose is soaked in the alkali liquor and generates a large amount of furan compounds, thereby polluting the resin.

Disclosure of Invention

the invention mainly aims at the problems that impurities in xylose solution are adsorbed by ion exchange resin and cannot be resolved by conventional desorbent, and the impurities are retained in the resin for a long time, so that the resin is polluted and the like in the conventional adsorption and desorption regeneration process of the ion exchange column in the long-term adsorption ion use process. In the technical scheme, through the application of the resuscitation agent, impurities in the ion exchange column are promoted to fall off, so that the condition that the exchange capacity of the resin is reduced after the resin is used for a long time is improved, the exchange multiple of the resin is increased to be close to the original level, and the service life of the resin is prolonged.

In order to achieve the technical purpose, the following technical scheme is proposed:

A recovery method of an ion exchange column used in xylose preparation comprises the following steps: injecting a resuscitation agent into the ion exchange column to be resuscitated at the flow rate of 5-10 m/h, resuscitating for more than 24h at the temperature of 40-45 ℃, and performing post-treatment to obtain the resuscitated ion exchange column.

Furthermore, the ion exchange column to be recovered is an ion exchange column with the ion exchange multiple reduced to 75-85% of the original ion exchange multiple (generally after the resin is used for 3-6 months), and the ion exchange capacity is reduced by 20-30% compared with the normal operation of the ion exchange column after the ion exchange column is regenerated by a desorbent (such as sodium hydroxide, hydrochloric acid and the like) and cleaning water in the prior art.

Further, the resuscitation agent comprises the following components in percentage by mass: 0.1-0.15% of bleaching powder, 1-1.5% of hydrogen peroxide, 7-8% of sodium chloride and 2-2.5% of sodium hydroxide.

Further, the content of available chlorine in the bleaching powder is 30-38%.

Further, the preparation method of the resuscitation agent comprises the following steps: adding bleaching powder, hydrogen peroxide, sodium chloride and sodium hydroxide into a preparation tank in sequence, and stirring for more than 1h for later use; after the resuscitation agent is prepared, the standing time cannot exceed 12 h.

Further, before injecting a resuscitation agent, pretreating an ion exchange column to be resuscitated, wherein the pretreatment comprises small backwashing, and specifically comprises the following steps: opening a drain valve in the middle of the ion exchange column, introducing cleaning water into the ion exchange column through an intermediate drain device, performing small backwashing for 5min at a flow speed of 10m/h, and washing off dirt accumulated on a fat pressing layer and the intermediate drain device during overfeeding operation; and finally, opening a water inlet valve at the upper part of the ion exchange column, and discharging accumulated water in the ion exchange column to the surface of the grease pressing layer to ensure that the grease pressing layer is in a state of not being soaked by water.

Further, the post-treatment comprises a small washing, specifically: opening a water inlet valve at the upper part of the ion exchange column, introducing cleaning water into the ion exchange column, and carrying out small forward washing at the flow speed of 20-30 m/h; and finally, opening a liquid discharge valve in the middle of the ion exchange column until the refraction of the solution in the liquid discharge valve is less than 1.

Further, the ion exchange column after recovery is detected according to the standard GB/T23532-2009 xylose, and the following results are obtained: the resin exchange capacity is increased by 30-50%, the water consumption is reduced by 30-40%, the discharging refraction is 7-8, the electric conductivity is lower than 500us/cm, and the light transmittance is higher than 90.

furthermore, the recovery ion exchange column has the exchange capacity weakened by more than 20%, large backwashing is carried out for 10-15 min (namely, the discharged liquid is clear and transparent) at the flow speed of 10-15 m/h, the resin backwashing development rate is ensured to be 50-80%, mechanical impurities and broken resin intercepted by the resin are taken away along with backwashing water flow, and the resin with normal particle size is prevented from being taken away by water; then, injecting a recovery agent into the ion exchange column at the flow rate of 10-20 m/h, and performing recovery treatment on the resin in the ion exchange column.

The wash water comprises deionized water.

A resuscitation system for an ion exchange column in xylose preparation comprises the ion exchange column, a cleaning water storage tank and a resuscitation agent storage tank, wherein the cleaning water storage tank is connected with the ion exchange column through a conveying pipe I, and the resuscitation agent storage tank is connected with the ion exchange column through a conveying pipe II; and control valves are arranged on the conveying pipe I and the conveying pipe II.

Furthermore, the conveying pipe I is connected with a water inlet valve and a liquid outlet valve on the ion exchange column, and the conveying pipe II is connected with a resuscitation agent inlet valve on the ion exchange column.

Furthermore, the ion exchange column comprises a tank body and a cavity arranged in the tank body, a water inlet valve and a resuscitation agent inlet valve are arranged at the upper part of the tank body, and a liquid discharge valve is arranged at the middle part of the tank body; resin is arranged in the cavity, and a grease pressing layer is arranged on the surface layer of the resin; and the middle part of the cavity is provided with an intermediate liquid drainage device, and the intermediate liquid drainage device and the liquid drainage valve form a passage.

Further, jar body upper portion still is equipped with feed inlet and radar level gauge mouth, and the bottom is equipped with the discharge gate, and jar internal feeding distributor that is equipped with, feeding distributor and feed inlet formation route.

Further, the ion exchange column is an ion exchange column filled with a D301 anion resin.

By adopting the technical scheme, the beneficial technical effects brought are as follows:

1) In the invention, mainly for the problem that the impurities in the xylose are absorbed by the ion exchange resin to cause the resin to be polluted, the arrangement of the resuscitation agent and the application thereof prompts the impurities in the ion exchange column to fall off and be removed, thereby realizing the resuscitation of the resin, improving the exchange multiple of the resin to the original level and prolonging the service life of the resin. The method is pertinently suitable for the process for preparing xylose by hydrolyzing hemicellulose, and effectively treats the interference of other impurities (such as furan compounds) generated in the recovery process of the ion exchange column on the ion exchange resin;

2) the invention has reasonable design and good resuscitation quality. In the recovery agent, bleaching powder is compatible with hydrogen peroxide and used for oxidizing residual furan impurities; and sodium chloride and sodium hydroxide are used for resin recovery. In the xylose preparation process, resin in an ion exchange column mainly adsorbs sulfate ions, organic acids and the like, 7-8% of sodium chloride solution is used to effectively replace the sulfate ions, the organic acid ions and the like in the resin with chloride ions, and then hydroxide ions in 2-2.5% of sodium hydroxide are used to replace the chloride ions, so that the problems that in the prior art, sodium hydroxide is directly used to recover the ion exchange column, and the sulfate ions, the organic acids and the like cannot be sufficiently replaced and fall off and the like are solved;

3) In the invention, the resin exchange capacity is increased by 30-50%, the cleaning frequency of the ion exchange column resin is reduced, and the service life of the resin is prolonged by 20-50%;

4) In the invention, based on the resuscitation agent and the resuscitation method, the available water amount for resuscitation process is reduced by 30-40%. The water quantity for flushing the resin in the ion exchange column is reduced, and water resource conservation is effectively realized;

5) In the invention, after the ion exchange column is resuscitated by the resuscitating agent, the light transmittance of the purified material is greatly improved, the discharged material refracts light to 7-8, the electrical conductivity is lower than 500us/cm, and the light transmittance is higher than 90;

6) In the invention, the sugar content in the discharged waste liquid in the recovery process is reduced, and more than 20 percent of COD in the discharged waste liquid in the recovery process is reduced;

7) In the invention, the resuscitation agent enters the ion exchange column to be resuscitated at the flow rate of 5-10 m/h, and the flow rate is limited, so that the resin layer is not disturbed, and the stability of the environment in the ion exchange column is ensured;

8) In the invention, before the resuscitating agent is injected, the ion exchange column to be resuscitated is pretreated, the pretreatment comprises small backwashing, the small backwashing washes away dirt accumulated on a grease pressing layer and an intermediate drainage device during overfeeding operation, and meanwhile, a branch drain pipe filter screen is dredged, the grease pressing layer is leveled and loosened, so that the preparation work is carried out for the resuscitating process, and the high efficiency and the high quality of the resuscitating process are ensured;

9) In the invention, after the ion exchange column is recovered, the ion exchange column is subjected to post-treatment, wherein the post-treatment comprises small washing, washing away residual recovery agent and recovery products such as a pressed lipid layer and the like, and the recovery effect of the ion exchange column is improved.

Drawings

FIG. 1 is a logical connection diagram of a resuscitation system of the present invention;

FIG. 2 is a connection block diagram of the present invention;

FIG. 3 is a schematic view of an ion exchange column according to the present invention;

Wherein, in the figure: 1. an ion exchange column, 2, a cleaning water storage tank, 3, a resuscitation agent storage tank, 4, conveying pipes I and 5, conveying pipes II and 6 and a control valve; 11. a tank body, 110, a water inlet valve, 111, a resuscitation agent inlet valve, 112, a liquid outlet valve, 113, a feed inlet, 114, a radar liquid level meter port, 115 and a discharge port; 12. cavity, 120, resin, 121, grease layer, 122, feed distributor.

Detailed Description

In the following, the technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.