阅读说明：本技术 一种邻苯二甲酸二异壬酯液相循环催化加氢的方法和装置 (Method and device for liquid-phase circulating catalytic hydrogenation of diisononyl phthalate ) 是由 卢巍 丁云杰 吕元 王涛 于婷婷 刁成际 马立新 于 2019-12-03 设计创作，主要内容包括：本发明涉及一种邻苯二甲酸二异壬酯(DINP)液相循环催化加氢的方法和装置。该方法将DINP在固定床反应器中催化加氢生成的产物粗环己烷1,2二甲酸二异壬酯,一部分作为稀释剂回流到加氢反应器,这部分粗DINCH先与原料DINP在一个液相混合器中混合,得到的稀释原料与略高于化学计量比的氢气在气液混合器中再次混合,得到的溶氢稀释原料进入加氢反应器,发生加氢反应；另一部分去下游精制单元经过汽提、碱洗、水洗和脱水四个步骤得到DINCH产品。该液相循环方法采用DINCH产品循环回加氢反应器,作为原料DINP的稀释剂,同时利用气液混合器提高氢气在稀释原料中的溶解效率,采用本发明提出的方法和装置,可以实现DINP转化率高于99.9％,DINCH选择性高于98％。(The invention relates to a method and a device for liquid-phase circulating catalytic hydrogenation of diisononyl phthalate (DINP). In the method, DINP is catalytically hydrogenated in a fixed bed reactor to generate a product, namely crude cyclohexane 1,2 diisononyl diformate, wherein one part of the crude DINP is used as a diluent and flows back to a hydrogenation reactor, the crude DINCH is firstly mixed with raw material DINP in a liquid phase mixer, the obtained diluted raw material is mixed with hydrogen slightly higher than the stoichiometric ratio again in a gas-liquid mixer, and the obtained dissolved hydrogen diluted raw material enters the hydrogenation reactor to generate hydrogenation reaction; the other part of the DINCH enters a downstream refining unit and is subjected to four steps of steam stripping, alkali washing, water washing and dehydration to obtain a DINCH product. The liquid phase circulation method adopts DINCH products to circulate back to the hydrogenation reactor as a diluent of the raw material DINP, and simultaneously improves the dissolution efficiency of hydrogen in the diluted raw material by using a gas-liquid mixer.)

1. The method for liquid-phase circulating catalytic hydrogenation of diisononyl phthalate is characterized by comprising the following steps:

(1) mixing a raw material diisononyl phthalate (DINP) from a raw material buffer tank with a reaction product crude cyclohexane 1,2 diisononyl phthalate (DINCH) (containing a small amount of by-products) from the reflux of a circulating pump in a liquid phase mixer, mixing the mixture with hydrogen from a new hydrogen compressor in a gas-liquid mixer in proportion, and then feeding the mixture into a hydrogenation reactor for hydrogenation reaction;

(2) separating the hydrogenated reaction product crude DINCH by a thermal high-pressure separator, wherein a part of a bottom liquid phase product flows back to a liquid phase mixer through a circulating pump to be mixed with the raw material DINP, and the other part of the bottom liquid phase product flows into a stripping tower of a downstream refining unit;

(3) after the gas phase product at the top is separated by the hot high-pressure separator, the gas phase product at the top is cooled by a water cooler and then is subjected to secondary separation by a cold high-pressure separator, the gas phase at the top of the cold high-pressure separator is discharged to a torch, and the liquid phase at the bottom is discharged to a light component storage tank;

(4) removing light components from the hydrogenated part of crude DINCH through a stripping tower, enabling the acid-containing DINCH at the bottom to enter an alkaline tower for deacidification, separating the light components at the top of the stripping tower by oil-water separation, removing an organic phase from a light component storage tank, and discharging a water phase to perform sewage treatment;

(6) the alkali-containing DINCH deacidified by the alkali washing tower enters a water washing tower to wash off redundant alkali;

(7) and (4) dewatering the washed water-containing DINCH in a dewatering tower to obtain a product DINCH, and conveying the product DINCH to a product tank.

2. The method of claim 1, wherein the ratio of feed DINP to the molar flow of hydrogen from the fresh hydrogen compressor is 1: 3-4, the mass ratio of the product crude DINCH refluxed to the liquid phase mixer to the product crude DINCH sent to the downstream stripping tower is 1: 0.05-0.3.

3. The method of claim 1, wherein the hydrogenation reactor is a trickle bed reactor, the operating temperature is 130-240 ℃, and the pressure is 2-16 MPa; the pressure of the hot high-pressure separator is 2-16 MPa, and the operating temperature is 120-240 ℃; the pressure of the cold high-pressure separator is 2-16 MPa, and the operating temperature is 20-40 ℃.

4. The method according to claim 1, wherein 3 to 5 catalyst beds are arranged in the hydrogenation reactor, and the catalyst beds comprise a protective agent layer, 1 to 2 low-activity high-stability layers and 1 to 2 high-activity layers from top to bottom; the protective agent is alumina ceramic ballOne or more of alumina foamed ceramic, activated carbon, silica gel and porous alumina carrier; the active component of the catalyst adopted by the low-activity high-stability layer and the high-activity layer is one or more of noble metals Pd, Pt and Ru, and the carrier is SiO₂、Al₂O₃One or more of SiC and active carbon; the active component load of the low-activity high-stability layer is 0.1-0.5%, the active component load of the high-activity layer is more than 0.5-1%, and the reaction material flows through the catalyst bed layer in the hydrogenation reactor from top to bottom.

5. The method of claim 1, wherein the temperature of the bottom of the stripping tower is 100-160 ℃, the temperature of the top of the stripping tower is 40-90 ℃, and the vacuum degree is-60-100 kPa; the temperature of the tower kettle of the dehydration tower is 140-160 ℃, and the vacuum degree is-60 to-100 kPa.

6. The method of claim 1, wherein the caustic tower is operated at a temperature of 40-90 ℃ and the caustic solution is Na₂CO₃、NaHCO₃And one or more of NaOH; the operation temperature of the water washing tower is 40-90 ℃.

7. An apparatus for the liquid-phase recycle continuous hydrogenation of DINP as described in any one of claims 1 to 6, wherein the apparatus comprises a hydrogenation reaction unit and a product purification unit;

the hydrogenation reaction unit comprises a hydrogenation reactor, a hot high-pressure separation tank connected with the bottom of the hydrogenation reactor, a circulating pump connected with a liquid phase outlet at the bottom of the hot high-pressure separation tank, a liquid phase mixer connected with an outlet of the circulating pump and a raw material buffer tank, and a gas-liquid mixer connected with an outlet of the liquid phase mixer and an outlet of a fresh hydrogen compressor, wherein an outlet of the gas-liquid mixer is connected with the top of the hydrogenation reactor; the product refining unit comprises a stripping tower, an alkaline washing tower, a water washing tower and a dehydrating tower which are sequentially connected in series.

8. The device according to claim 7, wherein more than 4 groups of gas distributors capable of breaking gas into millimeter-sized bubbles are sequentially arranged in the gas-liquid mixer from left to right, one end of each gas distributor is connected with a gas source, the other end of each gas distributor is provided with a gas outlet with 0.1-1 mm-diameter irregularly-distributed gas holes, the gas outlets are arranged below the liquid level, liquid flows through the gas-liquid mixer from left to right, a liquid baffling baffle is arranged between every two groups of distributors, and the structure can enhance the dissolution and dispersion of hydrogen in the liquid phase.

Technical Field

The invention relates to a method and a device for liquid-phase circulating catalytic hydrogenation of diisononyl phthalate (DINP), belonging to a reaction for preparing cyclohexane environment-friendly plasticizers by hydrogenation of benzene-containing plasticizers. The proposal of the technology promotes the development of the benzene-containing plasticizer in the existing PVC industry to the direction of low dissolution and low toxicity, and is beneficial to the cleanness and harmlessness of the industry. The product is widely suitable for producing soft PVC products such as food preservative films, shoes, non-slip mats, water pipes, wires and cables, and the like, and is particularly suitable for products requiring low toxicity and low dissolution, such as children toys, blood bags, intravenous transfusion tubes and the like.

Background

The plasticizer is an important component in PVC products, can increase the flexibility of plastics, and is widely used for filling and modifying PVC materials. The plasticizers used at present mainly include epoxy plasticizers represented by epoxidized soybean oil and phthalate plasticizers represented by diisooctyl phthalate (DOP). The o-benzene plasticizer has the best cost performance, so the o-benzene plasticizer is most widely applied, and the worldwide usage amount is more than 800 million tons every year. However, recent researches have found that the o-benzene plasticizer has poor stability in PVC, is easy to dissolve out and enter the environment, and causes a series of adverse effects. For example, entry into the human body via the digestive system, respiratory system, and skin contact, presents masked reproductive and developmental toxicities, such as the "plasticizer" event in taiwan, a negative example of the effects of ortho-benzene plasticizers on the human body. Therefore, Europe has already made regulations to prohibit the use of DOP plasticizers, and thus the gradual withdrawal of o-benzene plasticizers from the market is gradually reaching consensus in countries around the world.

Diisononyl phthalate (DINP), a plasticizer with superior properties to DOP, is mainly characterized by a lower mobility, making it more suitable for use in human contact. However, DINP has a certain safety risk even when a small amount of DINP is eluted due to the presence of a benzene ring structure. DINP is therefore located as "unclassified" in countries in the united states and europe, on the one hand because there is not yet a sufficient demonstration of the toxicity of DINP, and on the other hand represents a concern about the migration of its ortho-benzene components. Therefore, the benzene ring structure in the DINP is saturated into cyclohexane by adopting a hydrogenation means, namely the product of cyclohexane 1,2 diisononyl Diformate (DINCH) is synthesized, so that the benzene content in the product is reduced to be below 500ppm, and the superior product is lower than 100ppm, thereby fundamentally avoiding worrying about the benzene migration problem of the plasticizer, and really synthesizing the low-toxicity and pollution-free environment-friendly plasticizer product.

The prior DINCH technology prepared by hydrogenating DINP is mainly owned by BASF company, and a plurality of patents at home and abroad also disclose relevant catalyst and process technology. For example, chinese patent CN103130646B describes a process for producing DINCH by hydrogenating DINP, which is characterized in that a hydrogenation reactor adopts a batch still, and the subsequent steps of alkali washing and water washing are mainly completed by using a batch still reactor. Chinese patents CN102658182B, CN10698410A and CN110052266A disclose methods for preparing cyclohexane diformate catalysts by phthalate hydrogenation, but do not mention the reactor and its complement technology. Chinese patent CN110078617A describes a method for preparing cyclohexane diformate by catalytic hydrogenation of phthalate, which mentions that the process is implemented by using a continuous fixed bed reactor, but does not relate to a product refining process and a raw material/product recycling technology. U.S. Pat. No. 4,894646782 describes a process for preparing cyclohexanedicarboxylic acid esters by catalytic hydrogenation of phthalic acid esters, but does not involve recycling of the reaction products.

In fact, due to the highly exothermic nature of the DINP hydrogenation process, increasing the hydrogen recycle and diluting the feed DINP are both effective means to control the reaction temperature. The increase of the circulation volume of the hydrogen is simple and feasible, but the larger gas volume requires higher compression energy consumption on one hand, and the higher hydrogen-ester ratio causes a large amount of redundant gas phase to appear in the reactor on the other hand, so that the utilization rate of the hydrogen is lower. Therefore, the dilution of the DINP with the product DINCH is a reliable means at present. The method can not only utilize the high specific heat capacity of the liquid to absorb the heat of the hydrogenation reaction, but also reduce the hydrogen-ester ratio, increase the liquid holdup in the reactor and prolong the effective residence time of the reactants.

Disclosure of Invention

The invention aims to provide a method and a device for liquid-phase circulating catalytic hydrogenation of diisononyl phthalate (DINP), which mainly solve the problems of local hot spots caused by large reaction heat and difficult control of reaction temperature in the reaction process, avoid the generation of low-value byproducts such as isononane, acid and the like by excessive hydrogenation of products at high temperature, and improve the DINP conversion rate and DINCH selectivity. Meanwhile, a gas-liquid mixer capable of generating millimeter-scale bubbles is utilized to enhance the dissolving efficiency of hydrogen in reaction raw materials, so that the ratio of the hydrogen dissolved in the diluted raw materials to the raw material DINP is up to or higher than the stoichiometric ratio (3:1), a recycle hydrogen compressor can be omitted, and the purposes of reducing equipment investment and operating energy consumption are achieved.

In order to achieve the above object, with reference to fig. 1 and fig. 2, the technical solution adopted by the present invention specifically includes:

a DINP liquid phase circulation catalytic hydrogenation device is characterized by comprising a hydrogenation reaction unit and a product refining unit. The hydrogenation reaction unit comprises a hydrogenation reactor R-0101, a hot high-pressure separation tank V-0102 connected with the bottom of the hydrogenation reactor, a circulating pump P-0101 connected with a liquid phase outlet at the bottom of the hot high-pressure separation tank, a liquid phase mixer M-0101 connected with an outlet of the circulating pump and a raw material buffer tank V-0101, a gas-liquid mixer M-0102 connected with an outlet of the liquid phase mixer and an outlet of a new hydrogen compressor, and an outlet of the gas-liquid mixer is connected with the top of the hydrogenation reactor. The product refining unit comprises four parts, namely a stripping tower T-0101, an alkaline washing tower T-0102, a water washing tower T-0103 and a dehydrating tower T-0104. The inside gas distributor that is provided with the multiunit and can breaks into millimeter level bubble with gas of gas-liquid mixer M-0102, set up baffling baffle between every two sets of distributors, this structure can strengthen dissolving and the dispersion of hydrogen in the liquid phase.

A DINP liquid phase circulation catalytic hydrogenation method mainly comprises the following steps:

(1) raw material DINP from a raw material buffer tank V-0101 is mixed with crude DINCH (mainly DINCH containing a small amount of light components) from a circulating pump P-0101 in a liquid phase mixer M-0101 at a molar flow ratio of 0.05-0.3, then mixed with hydrogen from a new hydrogen compressor C-0101 in a gas-liquid mixer M-0102 at a molar flow ratio of 3-4 of hydrogen and DINP, and then fed into a hydrogenation reactor R-0101 for hydrogenation reaction. The operating temperature of the hydrogenation reactor is 130-240 ℃, and the pressure is 2-16 MPa.

(2) And after the hydrogenated reaction product flows out from an outlet of the R-0101, a liquid-phase product crude DINCH separated by a hot high-pressure separator V-0102 passes through a circulating pump P-0101, one part of the crude DINCH is mixed with the raw material DINP and hydrogen in a mixer M-0102, and the other part of the crude DINCH is sent to a downstream refining unit stripping tower T-0101. The operation temperature of the hot high-pressure separator V-0102 is 120-240 ℃, and the pressure is 2-16 MPa.

(3) And cooling a small amount of gas-phase products separated by the hot high-pressure separator V-0102 by a water cooler E-0103, cooling the high-pressure separator V-0103, removing a flare from the gas phase of the V-0103, and removing light components from the liquid phase of the V-0103 to recover the TK-0102. The operation temperature of the cold high-pressure separator is 20-40 ℃, and the pressure is 2-16 MPa.

(4) The reaction mixture is subjected to light component removal by a stripping tower T-0101 to become acid-containing DINCH, enters an alkaline washing tower T-0102 for deacidification, and the light component at the top of the stripping tower T-0101 is removed to obtain the TK-0102. The temperature of the kettle of the stripping tower is 100-160 ℃, the temperature of the top of the stripping tower is 40-90 ℃, and the vacuum degree is-60 to-100 kPa. The operating temperature of the alkaline washing tower is 40-90 ℃, and the alkali liquor is Na₂CO₃、NaHCO₃And NaOH.

(5) The alkali-containing DINCH deacidified by the T-0102 enters a water washing tower T-0103 to wash away redundant alkali. The operation temperature of the water washing tower is 40-90 ℃.

(6) And (3) dehydrating the washed water-containing DINCH in a dehydrating tower T-0104 to obtain a product DINCH in a product tank TK-0101. The temperature of the tower kettle of the dehydration tower T-0104 is 140-160 ℃, and the vacuum degree is-60 to-100 kPa.

The inside 3 ~ 5 catalyst bed layers that set up of hydrogenation ware is from last to being in proper order down for protective agent layer, 1 ~ 2 low activity high stability layer and 1 ~ 2 high active layer. Wherein the protective agent is one or more of alumina ceramic ball, alumina foamed ceramic, active carbon, silica gel and porous alumina carrier, the active component of the catalyst is one or more of noble metals Pd, Pt and Ru, and the carrier is SiO₂、Al₂O₃One or more of SiC and active carbon. The active component load of the low-activity high-stability layer is 0.1-0.5%, the active component load of the high-activity layer is more than 0.5-1%, and the reaction material flows through the catalyst bed layer in the hydrogenation reactor from top to bottom.

Because the process adopts a liquid phase circulation method, the concentration of reactants is low, the heat release is small, the liquid holdup in the reactor is large, the heat exchange efficiency is high, the problems of local hot spots caused by large reaction heat and difficult control of reaction temperature in the reaction process can be solved, low-value byproducts such as isononane, acid and the like generated by excessive hydrogenation of products at high temperature are avoided, and the DINP conversion rate and the DINCH selectivity are improved. Meanwhile, the process utilizes a gas-liquid mixer capable of generating millimeter-scale bubbles to enhance the dissolving efficiency of hydrogen in reaction raw materials, so that the ratio of the hydrogen dissolved in the diluted raw materials to the raw material DINP is up to or higher than the stoichiometric ratio (3:1), a recycle hydrogen compressor can be omitted, and the purposes of reducing equipment investment and operating energy consumption are achieved. By adopting the method and the device provided by the invention, the DINP conversion rate can be higher than 99.9%, and the DINCH selectivity is higher than 98%.

Drawings

FIG. 1 is a schematic diagram of the DINP liquid phase circulating catalytic hydrogenation DINCH production method of the device of the present invention V-0101: a raw material DINP buffer tank; v-0102: a hot high pressure knockout drum; v-0103: a cold high pressure knockout drum; r-0101: a hydrogenation reactor; m-0101: a liquid phase mixer; m-0102: a gas-liquid mixer; t-0101: a stripping column; t-0102: an alkaline washing tower; t-0103: washing the tower with water; t-0104: a dehydration tower; TK-0101: a product DINCH storage tank; TK-0102: a light component storage tank.

FIG. 2 is a schematic view of a gas-liquid separator apparatus according to the present invention.

1. A gas distribution nozzle; 2. baffle plate

Detailed Description

The present invention will be further described with reference to the following examples and drawings, but the present invention is not limited thereto.

Example 1

DINP flow 700kg/h, with a flow 2500kg/h from P-0101 in the reaction mixture in M-0101, into M-0102 and from the new hydrogen compressor C-0101 at a flow 116Nm³The hydrogen is mixed for h and enters the hydrogenation reactor R-0101 from the top. The operating temperature of R-0101 is 130 ℃, and the pressure is 16 MPa. The V-0102 bottom liquid phase reaction mixture is divided into two paths through P-0101, one path of the reaction mixture is mixed with the raw material DINP with the flow rate of 2100kg/h, and the other path of the reaction mixture is sent to a downstream refining unit stripping tower T-0101 with the flow rate of 700 kg/h. The vacuum degree of the stripping tower is-60 kPa, the temperature of the top of the tower is 90 ℃, and the temperature of the bottom of the tower is 160 ℃. The tower bottom liquid is sent to an alkaline washing tower T-0102, the operating temperature of the alkaline washing tower is 90 ℃, and the alkali liquor is Na₂CO₃And NaHCO₃. And (3) removing the oil phase at the top of the alkaline washing tower to a water washing tower T-0103, wherein the operation temperature of the water washing tower is 90 ℃. And (3) removing the oil phase at the top of the water washing tower to a dehydration tower T-0104, wherein the vacuum degree of the dehydration tower is-60 kPa, and the temperature of a tower kettle is 160 ℃. And removing the product TK-0101 from the product DINCH in the dehydration tower kettle, and removing the light component TK-0102 from the liquid phase in the top of the stripping tower and the V-0103 tank.

Analysis shows that the conversion rate of DINP is 99.91 percent, and the DINCH selectivity of the product is 99.2 percent.

Example 2

DINP flow 700kg/h, with a flow 2500kg/h from P-0101 in the reaction mixture in M-0101, into M-0102 and from the new hydrogen compressor C-0101 at a flow 116Nm³The hydrogen is mixed for h and enters the hydrogenation reactor R-0101 from the top. The operating temperature of R-0101 is 240 ℃, and the pressure is 2 MPa. The liquid phase reaction mixture at the bottom of V-0102 is divided into two paths by P-0101, one path of the reaction mixture with the flow rate of 1400kg/h is mixed with the raw material DINP, and the other path of the reaction mixture with the flow rate of 700kg/h enters a downstream refining unit stripping tower T-0101. The vacuum degree of the stripping tower is 80kPa, the temperature of the top of the tower is 80 ℃, and the temperature of the bottom of the tower is 140 ℃. The tower bottom liquid is sent to an alkaline washing tower T-0102, the operating temperature of the alkaline washing tower is 90 ℃, and the alkali liquor is Na₂CO₃And NaHCO₃. And (3) removing the oil phase at the top of the alkaline washing tower to a water washing tower T-0103, wherein the operation temperature of the water washing tower is 90 ℃. And (3) removing the oil phase at the top of the water washing tower to a dehydration tower T-0104, wherein the vacuum degree of the dehydration tower is-80 kPa, and the temperature of a tower kettle is 150 ℃. And removing the product TK-0101 from the product DINCH in the dehydration tower kettle, and removing the light component TK-0102 from the liquid phase in the top of the stripping tower and the V-0103 tank.

Analysis shows that the conversion rate of DINP is 99.99 percent, and the DINCH selectivity of the product is 98.1 percent.

Example 3

DINP flow 300kg/h, after mixing with the reaction mixture from P-0101 at a flow 6000kg/h in M-0101, into M-0102 and from the new hydrogen compressor C-0101 at a flow 70Nm³The hydrogen is mixed for h and enters the hydrogenation reactor R-0101 from the top. The operating temperature of R-0101 is 160 ℃, and the pressure is 16 MPa. The V-0102 bottom liquid phase reaction mixture is divided into two paths through P-0101, wherein one path has a flow of 6000kg/h, is mixed with the raw material DINP, and the other path has a flow of 300kg/h, and enters a downstream refining unit stripping tower T-0101. The vacuum degree of the stripping tower is-90 kPa, the temperature of the top of the tower is 50 ℃, and the temperature of the bottom of the tower is 130 ℃. The tower bottom liquid is sent to an alkaline washing tower T-0102, the operating temperature of the alkaline washing tower is 80 ℃, and the alkali liquor is Na₂CO₃And NaHCO₃. And (3) removing the oil phase at the top of the alkaline washing tower to a water washing tower T-0103, wherein the operation temperature of the water washing tower is 80 ℃. And (3) removing the oil phase at the top of the water washing tower to a dehydration tower T-0104, wherein the vacuum degree of the dehydration tower is-90 kPa, and the temperature of a tower kettle is 140 ℃. And removing the product TK-0101 from the product DINCH in the dehydration tower kettle, and removing the light component TK-0102 from the liquid phase in the top of the stripping tower and the V-0103 tank.

Analysis shows that the conversion rate of DINP is 99.99 percent, and the DINCH selectivity of the product is 99.1 percent.

Example 4

DINP flow 1000kg/h, after mixing with reaction mixture from P-0101 at flow 4000kg/h in M-0101, into M-0102 and from fresh hydrogen compressor C-0101 at flow 214Nm³The hydrogen is mixed for h and enters the hydrogenation reactor R-0101 from the top. The operating temperature of R-0101 is 190 deg.C, and the pressure is 12 MPa. The liquid phase reaction mixture at the bottom of the V-0102 is divided into two paths through the P-0101, one path has the flow rate of 4000kg/h, and is mixed with the raw material DINP, and the other path has the flow rate of 1000kg/h and enters a downstream refining unit stripping tower T-0101. The vacuum degree of the stripping tower is 100kPa, the temperature of the top of the stripping tower is 40 ℃, and the temperature of the bottom of the stripping tower is 100 DEG C. The tower bottom liquid is sent to an alkaline washing tower T-0102, the operating temperature of the alkaline washing tower is 90 ℃, and the alkali liquor is Na₂CO₃And NaHCO₃. And (3) removing the oil phase at the top of the alkaline washing tower to a water washing tower T-0103, wherein the operation temperature of the water washing tower is 90 ℃. And (3) removing the oil phase at the top of the water washing tower to a dehydration tower T-0104, wherein the vacuum degree of the dehydration tower is-100 kPa, and the temperature of a tower kettle is 140 ℃. And removing the product TK-0101 from the product DINCH in the dehydration tower kettle, and removing the light component TK-0102 from the liquid phase in the top of the stripping tower and the V-0103 tank.

Analysis shows that the conversion rate of DINP is 99.92%, and the DINCH selectivity of the product is 99.5%.

Example 5

DINP flow 1000kg/h, with a flow 5000kg/h from P-0101, after mixing in M-0101, into M-0102 and from the new hydrogen compressor C-0101 flow 214Nm³The hydrogen is mixed for h and enters the hydrogenation reactor R-0101 from the top. The operating temperature of R-0101 is 200 ℃, and the pressure is 16 MPa. The V-0102 bottom liquid phase reaction mixture is divided into two paths through P-0101, wherein one path has a flow rate of 5000kg/h, is mixed with the raw material DINP, and the other path has a flow rate of 1000kg/h, and enters a downstream refining unit stripping tower T-0101. The vacuum degree of the stripping tower is-90 kPa, the temperature of the top of the tower is 60 ℃, and the temperature of the bottom of the tower is 150 ℃. The tower bottom liquid is sent to an alkaline washing tower T-0102, the operating temperature of the alkaline washing tower is 90 ℃, and the alkali liquor is Na₂CO₃And NaHCO₃. And (3) removing the oil phase at the top of the alkaline washing tower to a water washing tower T-0103, wherein the operation temperature of the water washing tower is 90 ℃. And (3) removing the oil phase at the top of the water washing tower to a dehydration tower T-0104, wherein the vacuum degree of the dehydration tower is-90 kPa, and the temperature of a tower kettle is 150 ℃. And removing the product TK-0101 from the product DINCH in the dehydration tower kettle, and removing the light component TK-0102 from the liquid phase in the top of the stripping tower and the V-0103 tank.

Analysis shows that the conversion rate of DINP is 99.98 percent, and the DINCH selectivity of the product is 98.5 percent.

Example 6

DINP flow 700kg/h, with a flow 2500kg/h from P-0101, after mixing in M-0101, into M-0102 and from the new hydrogen compressor C-0101 at a flow 150Nm³The hydrogen is mixed for h and enters the hydrogenation reactor R-0101 from the top. The operating temperature of R-0101 is 200 ℃, and the pressure is 16 MPa. The V-0102 bottom liquid phase reaction mixture is divided into two paths through P-0101, one path has a flow rate of 2500kg/h, and is mixed with the raw material DINP, and the other path has a flow rate of 1000kg/h, and is sent to a downstream refining unit to be vaporizedAnd (5) extracting the tower T-0101. The vacuum degree of the stripping tower is 80kPa, the temperature of the top of the tower is 80 ℃, and the temperature of the bottom of the tower is 140 ℃. The tower bottom liquid is sent to an alkaline washing tower T-0102, the operating temperature of the alkaline washing tower is 40 ℃, and the alkali liquor is NaOH. And (3) removing the oil phase at the top of the alkaline washing tower to a water washing tower T-0103, wherein the operation temperature of the water washing tower is 90 ℃. And (3) removing the oil phase at the top of the water washing tower to a dehydration tower T-0104, wherein the vacuum degree of the dehydration tower is-80 kPa, and the temperature of a tower kettle is 150 ℃. And removing the product TK-0101 from the product DINCH in the dehydration tower kettle, and removing the light component TK-0102 from the liquid phase in the top of the stripping tower and the V-0103 tank.

Analysis shows that the DINP conversion rate is 99.93 percent, and the DINCH selectivity of the product is 98.5 percent.

Example 7

DINP flow 200kg/h, with a flow 2500kg/h from P-0101, after mixing in M-0101, into M-0102 and from the new hydrogen compressor C-0101 at a flow 150Nm³The hydrogen is mixed for h and enters the hydrogenation reactor R-0101 from the top. The operating temperature of R-0101 is 200 ℃, and the pressure is 16 MPa. The liquid phase reaction mixture at the bottom of the V-0102 is divided into two paths through the P-0101, one path of the reaction mixture is mixed with the raw material DINP with the flow rate of 2500kg/h, and the other path of the reaction mixture is sent to a downstream refining unit stripping tower T-0101 with the flow rate of 1000 kg/h. The vacuum degree of the stripping tower is 80kPa, the temperature of the top of the tower is 80 ℃, and the temperature of the bottom of the tower is 140 ℃. The tower bottom liquid is sent to an alkaline washing tower T-0102, the operating temperature of the alkaline washing tower is 40 ℃, and the alkali liquor is NaOH. And (3) removing the oil phase at the top of the alkaline washing tower to a water washing tower T-0103, wherein the operation temperature of the water washing tower is 90 ℃. And (3) removing the oil phase at the top of the water washing tower to a dehydration tower T-0104, wherein the vacuum degree of the dehydration tower is-80 kPa, and the temperature of a tower kettle is 150 ℃. And removing the product TK-0101 from the product DINCH in the dehydration tower kettle, and removing the light component TK-0102 from the liquid phase in the top of the stripping tower and the V-0103 tank.

Analysis shows that the conversion rate of DINP is 99.99 percent, and the DINCH selectivity of the product is 99.5 percent.