CN116099221A

CN116099221A - 1, 4-cyclohexanedimethanol purification device and purification method

Info

Publication number: CN116099221A
Application number: CN202310138796.6A
Authority: CN
Inventors: 邵建军; 郭榜立; 闫一伟; 徐建州; 张茂强; 于得水; 杜小龙; 崔世友; 董言纲
Original assignee: Jiangsu Honggang Petrochemical Co ltd
Current assignee: Jiangsu Honggang Petrochemical Co ltd
Priority date: 2023-02-21
Filing date: 2023-02-21
Publication date: 2023-05-12
Anticipated expiration: 2043-02-21
Also published as: CN116099221B

Abstract

The invention discloses a 1, 4-cyclohexanedimethanol purification device and a purification method, wherein the device comprises a dissolution treatment tank, the bottom of the dissolution treatment tank is communicated with a first-stage material pump through a material pipe, one end of the first-stage material pump, which is far away from the dissolution treatment tank, is communicated with a reduced-pressure rectification tank through a material pipe, the bottom of the reduced-pressure rectification tank is communicated with a second-stage material pump through a material pipe, one end of the second-stage material pump, which is far away from the reduced-pressure rectification tank, is communicated with a pressurizing rectification tank through a material pipe, and the device realizes the three-stage purification effect of dissolving crude pure 1, 4-cyclohexanedimethanol, namely reduced-pressure refined-pressurizing refined pure 1, 4-cyclohexanedimethanol, improves the purification rate of the 1, 4-cyclohexanedimethanol, and simultaneously detects the peak time and condition of the cis-trans isomer in the purified 1, 4-cyclohexanedimethanol so as to avoid influencing the heat resistance of the product.

Description

1, 4-cyclohexanedimethanol purification device and purification method

Technical Field

The invention relates to the technical field of 1, 4-cyclohexanedimethanol purification, in particular to a 1, 4-cyclohexanedimethanol purification device and a purification method.

Background

1, 4-cyclohexanedimethanol is alicyclic dihydric alcohol with symmetrical structure, contains 2 primary hydroxyl groups, has 2 structures of cis and trans, is an important basic chemical raw material, is solid wax-like at normal temperature and hard in texture at low temperature, is mainly used in the fields of novel polyester and polyurethane, is a frequently used chemical product in industrial production, and has wide application.

In the preparation process of 1, 4-cyclohexanedimethanol, in order to improve the purity of 1, 4-cyclohexanedimethanol, the purification treatment is needed to be carried out on the 1, 4-cyclohexanedimethanol, but most of the currently used purification devices are single rectification fraction purification treatment, and cannot integrate the actual operation and process detection combined means of dissolution impurity removal, solubility detection, partition temperature control, auxiliary hydrogenation, waste gas treatment and cis-trans isomer performance detection into a whole, so that the three-stage purification effect of 1, 4-cyclohexanedimethanol dissolution crude purity-decompression refined-pressurization refined purity is realized, the purification rate in the 1, 4-cyclohexanedimethanol is lower, the peak outlet time and the condition of the cis-trans isomer in the 1, 4-cyclohexanedimethanol cannot be known, and the heat resistance of the product cannot be influenced.

Disclosure of Invention

The invention aims to provide a 1, 4-cyclohexanedimethanol purification device and a purification method, which aim to solve the problems that most of the purification devices used at present in the background art are single rectification fraction purification treatment, and cannot integrate the actual operation and process detection of dissolution impurity removal, solubility detection, partition temperature control, auxiliary hydrogenation, waste gas treatment and cis-trans isomer performance detection into a whole, realize the three-stage purification effect of 1, 4-cyclohexanedimethanol dissolution crude purity-decompression refined purity-supercharging refined purity, reduce the purification rate of 1, 4-cyclohexanedimethanol, and have no understanding of the peak time and the situation of cis-trans isomers, and influence the heat resistance of products.

In order to achieve the above purpose, the present invention provides the following technical solutions: the utility model provides a 1, 4-cyclohexanedimethanol purification device, includes the dissolution processing jar, one side of dissolution processing jar is provided with the PLC switch board, the top of dissolution processing jar is linked together respectively and is had major ingredient charge door, ethylene glycol charge door and acetone auxiliary agent charge door, the bottom of dissolution processing jar is linked together through the material pipe and is had the one-level material pump, the one end that the dissolution processing jar was kept away from to the one-level material pump is linked together through the material pipe and is had the decompression rectifying tank, the one end that the decompression rectifying tank was kept away from to the second grade material pump is linked together through the material pipe and is had the pressure boost rectifying tank, the bottom intercommunication of pressure boost rectifying tank has the fraction discharge gate, the inner chamber of dissolution processing jar is provided with aeration impurity removing mechanism, be provided with subregion temperature control mechanism on dissolution processing jar, decompression rectifying tank and the pressure boost rectifying tank's one side is provided with hydrogen supply mechanism, the top of dissolution processing jar, decompression rectifying tank and pressure boost rectifying tank is provided with exhaust-gas treatment mechanism.

Preferably, the aeration impurity removing mechanism comprises a primary filter, the primary filter is communicated with one side of a primary material pump, which is close to a pressure reduction rectifying tank, one side of a secondary material pump, which is close to a pressure boost rectifying tank, is communicated with a secondary filter, one side of the top of the dissolution processing tank is fixedly connected with an aeration pump, an air outlet of the aeration pump is communicated with an aeration pipe, four ends of the aeration pipe are respectively provided with aeration holes, the periphery of the inner wall of the dissolution processing tank is respectively fixedly connected with a porous filter material, and a filter hole matched with the aeration holes is formed in an inner cavity of the porous filter material.

Preferably, the partition temperature control mechanism comprises a first temperature sensor, the first temperature sensor is embedded in one side of dissolving processing tank bottom, the opposite side of dissolving processing tank bottom is embedded with liquid sensor, the top of decompression rectifying tank and pressure boost rectifying tank is all embedded with second upper temperature sensor, the bottom of decompression rectifying tank and pressure boost rectifying tank is all embedded with second lower temperature sensor, one side in opposite directions of dissolving processing tank, decompression rectifying tank and pressure boost rectifying tank is provided with electric heating box and electric heating box's first cable is provided with and dissolves processing tank cover and establishes complex first heating frame, the inner chamber fixedly connected with of first heating frame and dissolves processing tank cooperation and use first electric heating ring, two wiring mouths of second cable and No. three cable of electric heating box all are provided with respectively through auxiliary cable with decompression rectifying tank and pressure boost rectifying tank top and bottom cover and establish complex second upper heating frame and second lower heating frame, two sets of upper heating frame and second heating frame that the second upper heating frame and third cable are all connected with second heating frame and pressure boost rectifying tank.

Preferably, the hydrogen supply mechanism comprises a hydrogen storage tank, the hydrogen storage tank is arranged on one side of the decompression rectifying tank and the pressurization rectifying tank, which is far away from the dissolution processing tank, a hydrogen outlet of the hydrogen storage tank is communicated with a pressurization air pump, a hydrogen outlet of the pressurization air pump is communicated with a three-way joint, two ends of the three-way joint are communicated with a branch pipe, the other end of the branch pipe is communicated with a buffer pipe which is communicated with the decompression rectifying tank and the pressurization rectifying tank, and two groups of buffer pipes are close to one ends of the decompression rectifying tank and the pressurization rectifying tank, and a pressure release valve is arranged at one end of the buffer pipe, which is close to the decompression rectifying tank and the pressurization rectifying tank.

Preferably, the exhaust treatment mechanism comprises an exhaust emission pipe, the exhaust emission pipe is communicated with the top of the dissolution treatment tank, the decompression rectification tank and the supercharging rectification tank, the exhaust emission pipe is far away from the top of the dissolution treatment tank, the decompression rectification tank and the supercharging rectification tank, the treatment tank is communicated with the inner cavity of the treatment tank, an activated carbon adsorption layer and a filter membrane layer are sequentially embedded in the inner cavity of the treatment tank from bottom to top, a tank cover is clamped at the top of the treatment tank, heat dissipation windows are formed in the periphery of the treatment tank, a rotating rod and a fan are rotationally connected at the center of the tank cover, and a turbulent fan is fixedly connected at the bottom of the rotating rod and used in cooperation with the heat dissipation windows.

Preferably, the aeration pipe adopts spiral design, the aperture of aeration hole is progressively reduced state distribution from top to bottom along the axis of aeration pipe in proper order, porous filter material is triangle equidistance state and adjacent contained angle is 120 along the axis of aeration pipe.

Preferably, the surfaces of the dissolution treatment tank, the decompression rectifying tank and the pressurization rectifying tank are respectively sleeved with a heat conduction pad matched with the first electric heating ring and the second electric heating ring.

Preferably, the guide fan and the turbulent flow fan are both in streamline design made of aluminum alloy materials, and the fan blades of the guide fan are larger than those of the turbulent flow fan and are four.

A method for purifying 1, 4-cyclohexanedimethanol, a 1, 4-cyclohexanedimethanol purification apparatus according to the above claims, comprising the steps of:

step one: firstly, injecting a to-be-treated solid waxy 1, 4-cyclohexanedimethanol main material into a dissolution treatment tank from a main material charging port, and then respectively injecting a glycol dissolver and an acetone auxiliary agent into the dissolution treatment tank from a glycol charging port and an acetone auxiliary agent charging port, wherein the molar ratio of the 1, 4-cyclohexanedimethanol main material to the glycol dissolver to the acetone auxiliary agent is 50:35:15, the electric heating box is controlled to be started by the PLC control cabinet, the electric heating box is electrified and heated to the first electric heating ring in the first heating frame through a first cable, heat generated by the first electric heating ring is conducted to the dissolution processing tank through the heat conduction pad, the solid waxy 1, 4-cyclohexanedimethanol main material in the dissolution processing tank is heated and dissolved, the temperature in the dissolution processing tank 1 is detected by the first temperature sensor, the temperature in the dissolution processing tank is kept between 20 ℃ and 25 ℃, the liquid sensor detects that the raw material in the dissolution processing tank is in a liquid state, meanwhile, the aeration pump is controlled to be started, high-pressure clean gas is applied to the aeration pipe, then the high-pressure clean gas is blown to the dissolved 1, 4-cyclohexanedimethanol main material, the ethylene glycol dissolving agent and the acetone auxiliary agent area through aeration holes distributed in a gradually decreasing mode from top to bottom, the high-pressure gas is mutually fused in the dissolution processing tank, preliminary purification reaction is carried out, the mixed solution of 1, 4-cyclohexanedimethanol is subjected to three groups of porous oil filtering materials after dissolution and mixed solution is subjected to the preliminary purification reaction, and the solution is subjected to the preliminary dissolution treatment, namely, the solution is subjected to the filtration treatment of the filtration of the crude filtration material is stopped at the maximum temperature of 1-25 ℃ after the three groups of the porous oil is removed, and the crude filtration material is completely removed;

Step two: when the dissolution treatment tank is heated to 20 ℃ and 25 ℃, a user correspondingly takes out a part of the crude and pure 1, 4-cyclohexanedimethanol solution which is preliminarily dissolved in the dissolution treatment tank in the first step as a sample, and then carries out sample separation treatment on the molar ratio of the main material of the 1, 4-cyclohexanedimethanol, the glycol dissolvent and the acetone auxiliary agent in the crude and pure solution sample, and the mixture is divided into five component samples, wherein the molar ratio of the main material of the 1, 4-cyclohexanedimethanol, the glycol dissolvent and the acetone auxiliary agent in the five component samples is respectively 70:25: 5. 60:30: 10. 50:35: 15. 40:40:20 and 30:45:25, analysis 70 by gas chromatograph/mass spectrometer: 25: 5. 60:30: 10. 50:35: 15. 40:40:20 and 30:45:25 analyzing liquid phase, solid phase and dissolution phenomena of the 1, 4-cyclohexanedimethanol main material, the ethylene glycol dissolver and the acetone auxiliary agent in the crude pure solution sample at 20 ℃ and 25 ℃;

step three: then controlling a primary material pump to carry out primary dissolution on the crude pure 1, 4-cyclohexanedimethanol solution in the dissolution treatment tank through a material pipe, finely filtering the crude pure 1, 4-cyclohexanedimethanol solution by a primary filter, then feeding the crude pure 1, 4-cyclohexanedimethanol solution into a decompression rectifying tank, controlling an electric heating box to be started by a PLC control cabinet and electrifying a junction box at the position of the decompression rectifying tank through a second cable, synchronously generating heat by a second upper heating frame and a second electric heating ring in a second lower heating frame which are distributed up and down in the decompression rectifying tank, synchronously heating the tank top and the tank bottom of the decompression rectifying tank correspondingly through a heat conduction pad, simultaneously carrying out partition detection on the tank top temperature and the tank bottom temperature of the decompression rectifying tank by a second upper temperature sensor and a second lower temperature sensor on the decompression rectifying tank, the top temperature and the bottom temperature of the decompression rectifying tank are kept between 180 ℃ and 210 ℃ and 200 ℃ to 230 ℃, the internal pressure of the decompression rectifying tank is kept between 0.8 MPa and 1MPa, meanwhile, a pressurizing air pump and a pressure release valve at the position of the decompression rectifying tank are controlled to be opened, hydrogen in a hydrogen storage tank is supplied into a branch pipe which leads to the direction of the decompression rectifying tank through a three-way joint by the pressurizing air pump, the hydrogen reaches the decompression rectifying tank through a buffer pipe, gas medium compensation is provided for the decompression rectifying reaction of the 1, 4-cyclohexanedimethanol crude pure solution until the top temperature and the bottom temperature of the decompression rectifying tank reach the highest value between 210 ℃ and 230 ℃ correspondingly, and then the decompression fraction purification work of the 1, 4-cyclohexanedimethanol crude pure solution in the decompression rectifying tank is completed, so that the 1, 4-cyclohexanedimethanol primary pure solution is obtained;

Step four: then the first-grade refined solution of 1, 4-cyclohexane dimethanol after the decompression fraction in the decompression rectifying tank is filtered by a second-grade filter through a second-grade material pump and then is fed into the supercharging rectifying tank, then the PLC control cabinet controls the electric heating box to be started and electrifies a junction box at the position of the supercharging rectifying tank through a third cable, the supercharging rectifying tank is distributed with a second upper heating frame and a second electric heating ring in a second lower heating frame up and down to synchronously generate heat, the tank top and the tank bottom of the supercharging rectifying tank are correspondingly and synchronously heated through a heat conduction pad, the tank top and the tank bottom temperature of the supercharging rectifying tank are detected in a partitioning way through a second upper temperature sensor and a second lower temperature sensor on the supercharging rectifying tank, so that the tank top temperature and the tank bottom temperature of the supercharging rectifying tank are kept between 200 ℃ to 230 ℃ and 220 ℃ to 250 ℃, the internal pressure of the pressurizing rectifying tank is maintained at 1-1.5MPa, then a pressurizing air pump and a pressure release valve at the position of the pressurizing rectifying tank are controlled to be opened, hydrogen in the hydrogen storage tank is fed into a branch pipe leading to the direction of the pressurizing rectifying tank by the pressurizing air pump through a three-way joint, the hydrogen reaches the pressurizing rectifying tank through a buffer pipe, gas medium compensation is provided for the pressurizing rectifying reaction of the 1, 4-cyclohexanedimethanol primary rectifying solution until the tank top temperature and the tank bottom temperature of the pressurizing rectifying tank reach the highest values at 230 ℃ and 250 ℃, pressurizing fraction purifying work of the 1, 4-cyclohexanedimethanol primary rectifying solution in the pressurizing rectifying tank is completed, the 1, 4-cyclohexanedimethanol secondary rectifying solution is obtained, and finally the purified 1, 4-cyclohexanedimethanol secondary rectifying solution is discharged to the next working procedure section through a fraction discharge port of the pressurizing rectifying tank;

Step five: in the process of sequentially dissolving and coarsely purifying the main material of 1, 4-cyclohexanedimethanol, namely, the primary purification and the secondary purification in the dissolving treatment tank, the decompression rectification tank and the supercharging rectification tank, the generated waste gas flows into the treatment tank from three waste gas discharge pipes, then the active carbon adsorption layer and the filter membrane layer sequentially carry out secondary filtration adsorption on impurities such as metal particles, harmful substances and the like in the waste gas generated in the dissolving treatment tank, the decompression rectification tank and the supercharging rectification tank, under the action of natural wind force, the natural wind force is captured by a guide fan above a tank cover, and a rotating rod is forced to drive a turbulent fan to synchronously rotate along with the guide fan in the same direction, and the turbulent fan rapidly discharges the waste gas purified gas after the secondary filtration to the outside from a radiating window;

step six: taking out part of the purified 1, 4-cyclohexanedimethanol secondary refined solution obtained in the step four as a sample, and respectively using a nonpolar SE-54 chromatographic column and a strong polar PEG-20M chromatographic column to carry out chromatographic analysis and detection on cis-trans isomer and purification rate in the 1, 4-cyclohexanedimethanol secondary refined solution sample, so that the cis-trans isomer in the purified 1, 4-cyclohexanedimethanol secondary refined solution meets the standard requirements, and the purified 1, 4-cyclohexanedimethanol in the purified 1, 4-cyclohexanedimethanol secondary refined solution meets 99.92 percent.

Compared with the prior art, the invention has the beneficial effects that:

in the invention, through arranging an aeration impurity removing mechanism, a primary filter and a secondary filter are respectively used for carrying out fine filtration impurity removal on residual impurities in a 1, 4-cyclohexanedimethanol crude pure solution and a 1, 4-cyclohexanedimethanol primary refined pure solution in a primary feeding process and a secondary feeding process, an aeration pump is used for providing an aeration source, then an aeration pipe, an aeration hole, a porous filter material and a filter hole are matched, the effects of accelerating dissolution and oil removal impurity removal are realized on a 1, 4-cyclohexanedimethanol main material, an ethylene glycol dissolving agent and an acetone auxiliary agent in a dissolution treatment tank, the raw material pretreatment effect of the main material and other two auxiliary agents is played, the subsequent purification work of the 1, 4-cyclohexanedimethanol is facilitated, a partition temperature control mechanism is arranged, an electric heating box is used for providing a heat source, a first temperature sensor and a liquid sensor are used for detecting the temperature and dissolution condition in the dissolution treatment tank, the two groups of second upper temperature sensors and two groups of second lower temperature sensors are used for respectively detecting the temperatures of the tank bottoms and the tank tops of the decompression rectifying tank and the pressurization rectifying tank in a partitioning way, the first heating frame and the first electric heating ring are used for realizing the heating and heating effect on the dissolution processing tank, the two groups of junction boxes, the second upper heating frame, the second lower heating frame and the second electric heating ring are used for respectively realizing the heating and heating effect on the tank bottoms and the tank tops of the decompression rectifying tank and the pressurization rectifying tank, the decompression refining-pressurization refining work of 1, 4-cyclohexanedimethanol is facilitated, the hydrogen supply mechanism is arranged, the hydrogen storage tank is used for providing a hydrogen source, the pressurization air pump is used for providing a conveying power source, the two groups of three-way connectors, the branch pipes, the buffer pipes and the pressure release valves are used for matching, the decompression rectifying tank and the pressurization rectifying tank are matched with 1, in the process of the pressure reduction purification-pressurization purification treatment of the 4-cyclohexanedimethanol, a hydrogen medium is provided, the pressure reduction purification-pressurization purification reaction speed of the 1, 4-cyclohexanedimethanol is accelerated, the pressure reduction purification-pressurization purification reaction quality of the 1, 4-cyclohexanedimethanol is improved, an exhaust gas treatment mechanism is arranged, the purification effect of the 1, 4-cyclohexanedimethanol, namely the dissolution crude purity-pressure reduction purification-pressurization purification effect of the tank cover, a radiating window, a rotating rod, a guide fan and a turbulent fan is realized by the combination of an exhaust gas discharge pipe, a treatment tank, an active carbon adsorption layer, a filter membrane layer, a tank cover, a cooling window, a rotating rod, a guide fan and a turbulent fan, the treatment effect of waste gas is realized, the environmental protection performance of the 1, 4-cyclohexanedimethanol in the purification treatment process is improved, the pollution to the surrounding environment is prevented, the impurity is removed by dissolution, the solubility detection, the partition temperature control, the auxiliary hydrogenation, the waste gas treatment and the forward and reverse isomer performance detection are integrated, the three-level purification effect of the 1, 4-cyclohexanedimethanol is realized, and the forward and the reverse heat resistance of the 1, 4-cyclohexanedimethanol in the purified product is prevented from being influenced by the abnormal detection of the forward and reverse isomer in the time after the peak purification process of the 1, 4-cyclohexanedimethanol.

Drawings

FIG. 1 is a schematic diagram of the structure of the present invention;

FIG. 2 is a side view of the structure of the present invention;

FIG. 3 is a rear elevational view of the structure of the present invention;

FIG. 4 is a partial cross-sectional view of the structure of the dissolution processing tank of the present invention;

FIG. 5 is a side view of the structure of the aeration impurity removing mechanism of the present invention;

FIG. 6 is an exploded view of a zoned temperature control mechanism of the present invention;

FIG. 7 is a cross-sectional exploded view of the exhaust treatment mechanism of the present invention;

FIG. 8 is a table of dissolution data for the main 1, 4-cyclohexanedimethanol feed, the glycol dissolution agent, and the acetone adjuvant in step two of the present invention;

FIG. 9 is a bar graph of dissolution data for the main 1, 4-cyclohexanedimethanol feed, glycol dissolution agent, and acetone adjuvant in step two of the present invention;

FIG. 10 is a line graph showing the peak of cis-trans isomer in the second-stage refined solution of 1, 4-cyclohexanedimethanol in step six of the present invention.

In the figure: 1. a dissolution treatment tank; 2. a PLC control cabinet; 3. a main material charging port; 4. a glycol feed inlet; 5. an acetone auxiliary agent charging port; 6. a first-stage material pump; 7. a decompression rectifying tank; 8. a secondary material pump; 9. a pressurized rectifying tank; 10. an aeration impurity removing mechanism; 101. a primary filter; 102. a secondary filter; 103. an aeration pump; 104. an aeration pipe; 105. aeration holes; 106. porous filter materials; 107. filtering holes; 11. a partition temperature control mechanism; 111. a first temperature sensor; 112. a liquid sensor; 113. a second upper temperature sensor; 114. a second lower temperature sensor; 115. an electric heating box; 116. a first heating rack; 117. a first electrical heating coil; 118. a junction box; 119. a second upper heating rack; 1110. a second lower heating rack; 1111. a second electric heating coil; 12. a hydrogen supply mechanism; 121. a hydrogen storage tank; 122. a booster air pump; 123. a three-way joint; 124. a branch pipe; 125. a buffer tube; 126. a pressure release valve; 13. an exhaust gas treatment mechanism; 131. an exhaust gas discharge pipe; 132. a treatment box; 133. an activated carbon adsorption layer; 134. a filter membrane layer; 135. a case cover; 136. a heat radiation window; 137. a rotating rod; 138. a fan; 139. a turbulent fan; 14. a heat conduction pad.

Description of the embodiments

The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.

Example 1

Referring to fig. 1 to 7, the present invention provides a technical solution: the 1, 4-cyclohexane dimethanol purification device comprises a dissolution treatment tank 1, one side of the dissolution treatment tank 1 is provided with a PLC control cabinet 2, the top of the dissolution treatment tank 1 is respectively communicated with a main material feed inlet 3, an ethylene glycol feed inlet 4 and an acetone auxiliary agent feed inlet 5, the bottom of the dissolution treatment tank 1 is communicated with a first-stage material pump 6 through a material pipe, one end of the first-stage material pump 6 far away from the dissolution treatment tank 1 is communicated with a reduced pressure rectifying tank 7 through a material pipe, the bottom of the reduced pressure rectifying tank 7 is communicated with a second-stage material pump 8 through a material pipe, one end of the second-stage material pump 8 far away from the reduced pressure rectifying tank 7 is communicated with a pressurizing rectifying tank 9 through a material pipe, the bottom of the pressurizing rectifying tank 9 is communicated with a fraction discharge port, the inner cavity of the dissolution treatment tank 1 is provided with an aeration impurity removing mechanism 10, by arranging an aeration impurity removing mechanism 101 and a second-stage filter 102, residual impurities in the 1, 4-cyclohexanedimethanol crude pure solution and the 1, 4-cyclohexanedimethanol primary refined pure solution in the primary feeding and secondary feeding processes are respectively subjected to fine filtration and impurity removal, an aeration source is provided by an aeration pump 103, then an aeration pipe 104, an aeration hole 105, a porous filter material 106 and a filter hole 107 are matched, the effects of accelerating dissolution and oil removal and impurity removal are realized on the 1, 4-cyclohexanedimethanol main material, an ethylene glycol dissolving agent and an acetone auxiliary agent in the dissolution treatment tank 1, the raw material pretreatment effect of the main material and other two auxiliary agents is achieved, the subsequent purification work of the 1, 4-cyclohexanedimethanol is facilitated, a partition temperature control mechanism 11 is arranged on the dissolution treatment tank 1, the decompression rectification tank 7 and the pressurization rectification tank 9, the partition temperature control mechanism 11 is arranged, the heat source is provided by an electric heating box 115, the first temperature sensor 111 and the liquid sensor 112, the temperature and dissolution condition in the dissolution treatment tank 1 are detected, the temperatures of the tank bottoms and the tank tops of the decompression rectifying tank 7 and the pressurization rectifying tank 9 are detected in a partitioning way by two groups of second upper temperature sensors 113 and two groups of second lower temperature sensors 114 respectively, the dissolution treatment tank 1 is heated and warmed by a first heating frame 116 and a first electric heating ring 117, the heating and warming effect is realized by two groups of junction boxes 118, a second upper heating frame 119, a second lower heating frame 1110 and a second electric heating ring 1111 respectively, the tank bottoms and the tank tops of the decompression rectifying tank 7 and the pressurization rectifying tank 9 are heated and warmed respectively, the decompression rectifying-pressurization rectifying treatment work of 1, 4-cyclohexanedimethanol is facilitated, one sides of the decompression rectifying tank 7 and the pressurization rectifying tank 9 are provided with a hydrogen supply mechanism 12, a hydrogen storage tank 121 is provided with a hydrogen supply mechanism 12, the pressurizing air pump 122 provides a conveying power source, and then two groups of three-way connectors 123, branch pipes 124, buffer pipes 125 and pressure release valves 126 are matched to provide a hydrogen medium in the process of performing pressure reduction purification-pressurizing purification treatment on 1, 4-cyclohexanedimethanol by the pressure reduction rectification tank 7 and the pressurizing rectification tank 9, so that the pressure reduction purification-pressurizing purification reaction speed of the 1, 4-cyclohexanedimethanol is accelerated, the pressure reduction purification-pressurizing purification reaction quality of the 1, 4-cyclohexanedimethanol is improved, the tops of the dissolution treatment tank 1, the pressure reduction rectification tank 7 and the pressurizing rectification tank 9 are provided with an exhaust gas treatment mechanism 13, and the exhaust gas treatment mechanism 13 is arranged to realize the matching of the dissolution treatment tank 1, the pressure reduction rectification tank and the pressurizing rectification tank 9 by the exhaust gas discharge pipes 131, the treatment tank 132, the active carbon adsorption layer 133, the filter membrane layer 134, the tank cover 135, the heat dissipation window 136, the rotating rod 137, the guide fan 138 and the turbulent fan 139, the treatment effect of waste gas generated during each stage of reaction in the decompression rectifying tank 7 and the pressurization rectifying tank 9 is improved, the environmental protection performance in the purification treatment process of the 1, 4-cyclohexanedimethanol is improved, the pollution to the surrounding environment is avoided, the combination means of the actual operation and the process detection integrating the dissolution impurity removal, the solubility detection, the partition temperature control, the auxiliary hydrogenation, the waste gas treatment and the cis-trans isomer performance detection are adopted, the three-stage purification effect of the 1, 4-cyclohexanedimethanol dissolution crude purity-decompression refined purity-pressurization refined purity is realized, the purification rate of the 1, 4-cyclohexanedimethanol is improved, the peak time and the condition of the cis-trans isomer in the purified 1, 4-cyclohexanedimethanol are detected and known, and the influence on the heat resistance of the product caused by the abnormal occurrence of the cis-trans isomer in the purified 1, 4-cyclohexanedimethanol is avoided.

Example 2

Referring to fig. 1 to 10, the present invention provides a technical solution: the 1, 4-cyclohexane dimethanol purification device comprises a dissolution treatment tank 1, one side of the dissolution treatment tank 1 is provided with a PLC control cabinet 2, the top of the dissolution treatment tank 1 is respectively communicated with a main material feed inlet 3, an ethylene glycol feed inlet 4 and an acetone auxiliary agent feed inlet 5, the bottom of the dissolution treatment tank 1 is communicated with a first-stage material pump 6 through a material pipe, one end of the first-stage material pump 6 far away from the dissolution treatment tank 1 is communicated with a decompression rectifying tank 7 through a material pipe, the bottom of the decompression rectifying tank 7 is communicated with a second-stage material pump 8 through a material pipe, one end of the second-stage material pump 8 far away from the decompression rectifying tank 7 is communicated with a pressurizing rectifying tank 9 through a material pipe, the bottom of the pressurizing rectifying tank 9 is communicated with a fraction discharge port, the inner cavity of the dissolution treatment tank 1 is provided with an aeration impurity removing mechanism 10, the aeration impurity removing mechanism 10 comprises a first-stage filter 101, the first-stage filter 101 is communicated with one side of the first-stage material pump 6 near the decompression rectifying tank 7, the secondary material pump 8 is communicated with a secondary filter 102 near one side of the pressurizing rectifying tank 9, one side of the top of the dissolution processing tank 1 is fixedly connected with an aeration pump 103, the air outlet of the aeration pump 103 is communicated with an aeration pipe 104, the aeration pipe 104 adopts a spiral design, aeration holes 105 are formed at four ends of the aeration pipe 104, porous filter materials 106 are fixedly connected to the periphery of the inner wall of the dissolution processing tank 1, the pore diameters of the aeration holes 105 are distributed in a gradual decreasing state from top to bottom along the central axis of the aeration pipe 104, filter holes 107 matched with the aeration holes 105 are formed in the inner cavity of the porous filter materials 106, the porous filter materials 106 are in a triangular equidistant state along the central axis of the aeration pipe 104, the adjacent included angle is 120 degrees, the distribution uniformity of the porous filter materials 106 is improved, the impurity removal and filtration work of the filter holes 107 is facilitated, and 1, 4-cyclohexanedimethanol main materials in the dissolution processing tank 1, the ethylene glycol dissolvent and the acetone auxiliary agent are subjected to comprehensive aeration mixing treatment, an aeration impurity removing mechanism 10 is arranged, a primary filter 101 and a secondary filter 102 are respectively used for carrying out fine filtration impurity removal on residual impurities in a 1, 4-cyclohexanedimethanol crude pure solution and a 1, 4-cyclohexanedimethanol primary pure solution in a primary feeding process and a secondary feeding process, an aeration pump 103 is used for providing an aeration source, then an aeration pipe 104, an aeration hole 105, a porous filter material 106 and a filter hole 107 are matched, the effects of accelerating dissolution and oil removal impurity removal are realized on a 1, 4-cyclohexanedimethanol main material, the ethylene glycol dissolvent and the acetone auxiliary agent in a dissolution treatment tank 1, the raw material pretreatment effect of the main material and other two auxiliary agents is played, the subsequent purification work of the 1, 4-cyclohexanedimethanol is facilitated, a partition temperature control mechanism 11 is arranged on the dissolution treatment tank 1, a decompression rectification tank 7 and a pressurization rectification tank 9, the partition temperature control mechanism 11 comprises a first temperature sensor 111, the first temperature sensor 111 is embedded at one side of the bottom of the dissolution processing tank 1, a liquid sensor 112 is embedded at the other side of the bottom of the dissolution processing tank 1, a second upper temperature sensor 113 is embedded at the tops of the decompression rectifying tank 7 and the pressurization rectifying tank 9, a second lower temperature sensor 114 is embedded at the bottoms of the decompression rectifying tank 7 and the pressurization rectifying tank 9, an electric heating box 115 is arranged at one side of the dissolution processing tank 1, the decompression rectifying tank 7 and the pressurization rectifying tank 9 opposite to each other, a first heating frame 116 which is covered and matched with the dissolution processing tank 1 is arranged on a first cable of the electric heating box 115, a first electric heating ring 117 which is matched with the dissolution processing tank 1 is fixedly connected with the inner cavity of the first heating frame 116, the second cable and the third cable of the electric heating box 115 are respectively provided with a junction box 118, two junction ports of the junction box 118 are respectively provided with a second upper heating frame 119 and a second lower heating frame 1110 which are covered and matched with the top and the bottom of the vacuum rectification tank 7 and the pressurizing rectification tank 9 through auxiliary cables, the inner cavities of the two groups of second upper heating frames 119 and the second lower heating frame 1110 are fixedly connected with second electric heating rings 1111 which are matched with the vacuum rectification tank 7 and the pressurizing rectification tank 9, the surfaces of the dissolution treatment tank 1, the vacuum rectification tank 7 and the pressurizing rectification tank 9 are respectively sleeved with a heat conduction pad 14 which is matched with the first electric heating ring 117 and the second electric heating ring 1111, the heat conduction speed is accelerated, the partition heating operation of the dissolution treatment tank 1, the vacuum rectification tank 7 and the pressurizing rectification tank 9 is facilitated, a partition heating operation is provided by the electric heating box 115 through the arrangement of a partition temperature control mechanism 11, the first temperature sensor 111 and the liquid sensor 112 are used for detecting the temperature and the dissolution condition in the dissolution treatment tank 1, the two groups of second upper temperature sensors 113 and the two groups of second lower temperature sensors 114 are used for respectively detecting the tank bottom and the tank top temperatures of the reduced pressure rectifying tank 7 and the pressurized rectifying tank 9 in a partitioning way, the first heating frame 116 and the first electric heating ring 117 are used for realizing the heating and temperature rising effect on the dissolution treatment tank 1, the two groups of junction boxes 118, the second upper heating frame 119, the second lower heating frame 1110 and the second electric heating ring 1111 are used for respectively realizing the heating and temperature rising effect on the tank bottom and the tank top of the reduced pressure rectifying tank 7 and the pressurized rectifying tank 9, the reduced pressure rectifying tank 7 and the pressurized rectifying tank 9 are respectively beneficial to the reduced pressure rectifying-pressurized rectifying treatment work of 1, 4-cyclohexanedimethanol, one side of the reduced pressure rectifying tank 7 and the pressurized rectifying tank 9 is provided with the hydrogen supply mechanism 12, the hydrogen supply mechanism 12 comprises a hydrogen storage tank 121, the hydrogen storage tank 121 is arranged at one side of the decompression rectifying tank 7 and the pressurization rectifying tank 9 far away from the dissolution processing tank 1, a hydrogen outlet of the hydrogen storage tank 121 is communicated with a pressurization air pump 122, a hydrogen outlet of the pressurization air pump 122 is communicated with a three-way joint 123, two ends of the three-way joint 123 are both communicated with a branch pipe 124, the other end of the branch pipe 124 is communicated with a buffer pipe 125 which is communicated with the decompression rectifying tank 7 and the pressurization rectifying tank 9, one ends of the two groups of buffer pipes 125 close to the decompression rectifying tank 7 and the pressurization rectifying tank 9 are provided with pressure release valves 126, by arranging the hydrogen supply mechanism 12, the hydrogen storage tank 121 provides a hydrogen source, the pressurization air pump 122 provides a conveying power source, and then, by the cooperation of the two groups of the three-way joint 123, the branch pipe 124, the buffer pipe 125 and the pressure release valves 126, in the decompression rectifying process of the decompression rectifying tank 7 and the pressurization rectifying tank 9 to 1, 4-cyclohexane dimethanol, providing hydrogen medium, accelerating the reaction speed of decompression rectification and pressurization rectification of 1, 4-cyclohexanedimethanol, improving the reaction quality of decompression rectification and pressurization rectification of 1, 4-cyclohexanedimethanol, arranging an exhaust gas treatment mechanism 13 at the top of a dissolution treatment tank 1, a decompression rectification tank 7 and a pressurization rectification tank 9, wherein the exhaust gas treatment mechanism 13 comprises an exhaust gas discharge pipe 131, the exhaust gas discharge pipe 131 is communicated with the top of the dissolution treatment tank 1, the decompression rectification tank 7 and the pressurization rectification tank 9, one end of the exhaust gas discharge pipe 131 far away from the dissolution treatment tank 1, the decompression rectification tank 7 and the pressurization rectification tank 9 is communicated with a treatment tank 132, the inner cavity of the treatment tank 132 is sequentially embedded with an active carbon adsorption layer 133 and a filter membrane layer 134 from bottom to top, a tank cover 135 is clamped at the top of the treatment tank 132, windows 136 are arranged on the periphery of the treatment tank 132 close to the tank cover 135, the center of the box cover 135 is rotationally connected with a rotating rod 137, the top of the rotating rod 137 is fixedly connected with a guide fan 138, the bottom of the rotating rod 137 is fixedly connected with a turbulent flow fan 139 matched with the radiating window 136, the guide fan 138 and the turbulent flow fan 139 are of streamline design made of aluminum alloy materials, the fan blades of the guide fan 138 are larger than those of the turbulent flow fan 139 and are four, the weight of the guide fan 138 and the turbulent flow fan 139 is reduced, the rotating speeds of the guide fan 138 and the turbulent flow fan 139 are accelerated, and the exhaust gas treatment mechanism 13 is arranged, so that the exhaust gas treatment effect of waste gas generated during all-stage reactions in the dissolution treatment tank 1, the decompression rectification tank 7 and the pressurization rectification tank 9 is realized by the matching of the exhaust gas discharge pipe 131, the treatment tank 132, the active carbon adsorption layer 133, the filter membrane layer 134, the box cover 135, the radiating window 136, the rotating rod 137, the guide fan 138 and the turbulent flow fan 139, the treatment effect of the waste gas generated during all-stage reactions in the decompression rectification tank 7 and the pressurization rectification tank 9 is improved, and the environmental protection during the purification treatment of 1, and the pollution to the surrounding environment is prevented;

A method for purifying 1, 4-cyclohexanedimethanol according to the above-mentioned 1, 4-cyclohexanedimethanol purification device comprises the following steps:

step one: firstly, a user injects a main material of the solid waxy 1, 4-cyclohexanedimethanol to be treated into a dissolution treatment tank 1 from a main material feed inlet 3, and then respectively injects a glycol dissolver and an acetone auxiliary agent into the dissolution treatment tank 1 from a glycol feed inlet 4 and an acetone auxiliary agent feed inlet 5, wherein the mol ratio of the main material of the 1, 4-cyclohexanedimethanol, the glycol dissolver and the acetone auxiliary agent is 50:35:15, the PLC control cabinet 2 controls the electric heating box 115 to be started and the first electric heating ring 117 in the first heating frame 116 is electrified to heat through a first cable, the heat generated by the first electric heating ring 117 is conducted into the dissolution processing tank 1 through the heat conduction pad 14, the solid waxy 1, 4-cyclohexanedimethanol main material in the dissolution processing tank 1 is heated and dissolved, the temperature in the dissolution processing tank 1 is detected by the first temperature sensor 111, the temperature in the dissolution processing tank 1 is kept between 20 ℃ and 25 ℃, the liquid sensor 112 detects that the raw material in the dissolution processing tank 1 is in a liquid state, meanwhile, the aeration pump 103 is controlled to be started and high-pressure clean gas is applied into the aeration pipe 104, then the high-pressure clean gas is blown into the dissolved 1, 4-cyclohexanedimethanol main material, the ethylene glycol dissolving agent and the acetone auxiliary agent area through the aeration holes 105 distributed in a gradually decreasing state from top to bottom, the high-pressure clean gas is mutually fused in the dissolution processing tank 1, and primary purification reaction is generated, the mixed 1, 4-cyclohexanedimethanol is heated to the highest temperature is reached to the three-step-by the porous filtration material 1, and the primary dissolution processing solution is stopped, and the mixed 1, the mixed solution is purified, and the primary dissolution is removed from the primary dissolution processing solution is carried out at the porous 1, the porous filtration material is heated, the porous filtration material 1 and the porous filtration material is removed, the primary filtration material is at the primary filtration material 1 and the filtration material is removed, and the primary filtration material is removed from the primary filtration material 1;

Step two: when the dissolution treatment tank 1 is heated to 20 ℃ and 25 ℃, a user correspondingly takes out a part of the crude and pure 1, 4-cyclohexanedimethanol solution which is preliminarily dissolved in the dissolution treatment tank 1 in the first step as a sample, and then carries out sample separation treatment on the molar ratio of the main material of the 1, 4-cyclohexanedimethanol, the glycol dissolver and the auxiliary agent of the acetone in the crude and pure solution sample, and the mixture is divided into five component samples, wherein the molar ratio of the main material of the 1, 4-cyclohexanedimethanol, the glycol dissolver and the auxiliary agent of the acetone in the five component samples is respectively 70:25: 5. 60:30: 10. 50:35: 15. 40:40:20 and 30:45:25, analysis 70 by gas chromatograph/mass spectrometer: 25: 5. 60:30: 10. 50:35: 15. 40:40:20 and 30:45:25 analyzing liquid phase, solid phase and dissolution phenomena of the 1, 4-cyclohexanedimethanol main material, the ethylene glycol dissolver and the acetone auxiliary agent in the crude pure solution sample at 20 ℃ and 25 ℃; as can be seen from fig. 8, the molar ratio of the main material of 1, 4-cyclohexanedimethanol, the glycol dissolvent and the acetone auxiliary agent in the crude pure solution sample is 50:35:15, the liquid phase and the solid phase have the highest values and are uniformly dissolved, and as can be seen from fig. 9, the molar ratio of the main material of 1, 4-cyclohexanedimethanol, the glycol dissolver and the acetone auxiliary agent in the crude pure solution sample is 50:35:15, the solubility of the main material and the two auxiliary materials is optimal, and the solubility is close to 100%;

Step three: then the primary material pump 6 is controlled to carry out primary dissolution on the crude pure 1, 4-cyclohexanedimethanol solution in the dissolution treatment tank 1 through a material pipe, the crude pure 1, 4-cyclohexanedimethanol solution is fed into the reduced pressure rectification tank 7 after being filtered by the primary filter 101, then the PLC control cabinet 2 controls the electric heating box 115 to be opened and is electrified to the junction box 118 at the position of the reduced pressure rectification tank 7 through a second cable, the second upper heating frame 119 and the second lower heating ring 1111 in the second lower heating frame 1110 which are distributed up and down in the reduced pressure rectification tank 7 synchronously generate heat, the tank top and the tank bottom of the reduced pressure rectification tank 7 are synchronously heated correspondingly through the heat conduction pad 14, meanwhile, the temperatures of the tank top and the tank bottom of the reduced pressure rectification tank 7 are detected in a partitioning way through the second upper temperature sensor 113 and the second lower temperature sensor 114 on the reduced pressure rectification tank 7, maintaining the tank top temperature and the tank bottom temperature of the vacuum rectification tank 7 between 180 ℃ and 210 ℃ and 200 ℃ to 230 ℃ and maintaining the internal pressure of the vacuum rectification tank 7 between 0.8 MPa and 1MPa, simultaneously controlling the pressurizing air pump 122 and the pressure release valve 126 at the position of the vacuum rectification tank 7 to be opened, feeding the hydrogen in the hydrogen storage tank 121 into the branch pipe 124 leading to the direction of the vacuum rectification tank 7 through the three-way joint 123 by the pressurizing air pump 122, and feeding the hydrogen into the vacuum rectification tank 7 through the buffer pipe 125 to provide gas medium compensation for the vacuum rectification reaction of the 1, 4-cyclohexanedimethanol crude pure solution until the tank top temperature and the tank bottom temperature of the vacuum rectification tank 7 reach the highest values between 210 ℃ and 230 ℃ correspondingly, and completing the vacuum fraction purification work of the 1, 4-cyclohexanedimethanol crude pure solution in the vacuum rectification tank 7 to obtain the 1, 4-cyclohexanedimethanol primary pure solution;

Step four: then the 1, 4-cyclohexane dimethanol primary refined solution after the vacuum distillation in the vacuum rectification tank 7 is filtered by the secondary filter 102 through the secondary material pump 8 and then is fed into the pressurizing rectification tank 9, then the PLC control cabinet 2 controls the electric heating box 115 to be opened and the junction box 118 at the position of the pressurizing rectification tank 9 is electrified through a third cable, the pressurizing rectification tank 9 distributes the second upper heating frame 119 and the second electric heating ring 1111 in the second lower heating frame 1110 up and down to synchronously generate heat, synchronously heats the tank top and the tank bottom of the pressurizing rectification tank 9 correspondingly through the heat conduction pad 14, simultaneously carries out partition detection on the temperature of the tank top and the tank bottom of the pressurizing rectification tank 9 through the second upper temperature sensor 113 and the second lower temperature sensor 114 on the pressurizing rectification tank 9, so that the tank top temperature and the tank bottom temperature of the pressurizing rectification tank 9 are kept between 200 ℃ and 230 ℃ and 220 ℃ and 250 ℃, and the internal pressure of the pressurizing and rectifying tank 9 is maintained at 1-1.5MPa, then the pressurizing air pump 122 and the pressure release valve 126 at the position of the pressurizing and rectifying tank 9 are controlled to be opened, the hydrogen in the hydrogen storage tank 121 is supplied into the branch pipe 124 leading to the direction of the pressurizing and rectifying tank 9 by the pressurizing air pump 122 through the three-way joint 123, the hydrogen reaches the pressurizing and rectifying tank 9 through the buffer pipe 125, the pressurizing and rectifying reaction of the primary pure solution of the 1, 4-cyclohexanedimethanol is provided with gas medium compensation until the tank top temperature and the tank bottom temperature of the pressurizing and rectifying tank 9 reach the highest values at 230 ℃ and 250 ℃ correspondingly, the pressurizing fraction purifying work of the primary pure solution of the 1, 4-cyclohexanedimethanol in the pressurizing and rectifying tank 9 is completed, the secondary pure solution of the 1, 4-cyclohexanedimethanol is obtained, and finally the primary purified 1 is obtained, the 4-cyclohexanedimethanol secondary refined solution is discharged to the next working procedure section from a fraction discharge port of a pressurizing rectifying tank 9;

Step five: in the process of sequentially dissolving and coarsely purifying the main material of 1, 4-cyclohexanedimethanol, namely, the first-stage fine purification and the second-stage fine purification in the dissolving treatment tank 1, the decompression rectification tank 7 and the supercharging rectification tank 9, the generated waste gas flows into the treatment tank 132 through three waste gas discharge pipes 131, then the impurities such as metal particles and harmful substances in the waste gas generated in the dissolving treatment tank 1, the decompression rectification tank 7 and the supercharging rectification tank 9 are subjected to secondary filtration adsorption through an active carbon adsorption layer 133 and a filter membrane layer 134 in sequence, and under the action of natural wind force, the natural wind force is captured through a guide fan 138 above a tank cover 135, and a rotating rod 137 is forced to drive a turbulent fan 139 to synchronously rotate along with the guide fan 138 in the same direction, so that the turbulent fan 139 can rapidly discharge the waste gas purified by secondary filtration from a radiating window 136 to the outside;

step six: taking out part of the purified 1, 4-cyclohexanedimethanol secondary refined solution obtained in the step four as a sample, and respectively using a nonpolar SE-54 chromatographic column and a strong polar PEG-20M chromatographic column to carry out chromatographic analysis and detection on cis-trans isomer and purification rate in the 1, 4-cyclohexanedimethanol secondary refined solution sample, so that the cis-trans isomer in the purified 1, 4-cyclohexanedimethanol secondary refined solution meets the standard requirements, and the purified 1, 4-cyclohexanedimethanol in the purified 1, 4-cyclohexanedimethanol secondary refined solution meets 99.92 percent. As can be seen from FIG. 10, the cis-trans isomer in the 1, 4-cyclohexanedimethanol secondary purified solution sample showed prominent chromatographic performance in both the nonpolar SE-54 chromatographic column and the strongly polar PEG-20M chromatographic column, wherein the cis-trans isomer in the 1, 4-cyclohexanedimethanol secondary purified solution sample showed peak at 9.88min and 12.56min, respectively, the cis-trans isomer in the 1, 4-cyclohexanedimethanol secondary purified solution sample showed peak at 13.76min and 16.08min, respectively, when the strongly polar PEG-20M chromatographic column was analyzed, and the cis-trans isomer in the three-time purified 1, 4-cyclohexanedimethanol secondary purified solution obtained in the fourth step showed peak at 13.76min and 16.08min, respectively, as can be seen from the detection results, the method is characterized in that the method is a trans-isomer first-out peak, so that the purification requirement of the 1, 4-cyclohexanedimethanol after the second-stage fine purification meets or even exceeds the standard requirement, and the method adopts the combination means of the actual operation and process detection integrating the dissolution impurity removal, the solubility detection, the partition temperature control, the auxiliary hydrogenation, the waste gas treatment and the cis-trans isomer performance detection, thereby realizing the three-stage purification effect of 1, 4-cyclohexanedimethanol dissolution crude purity-decompression fine purity-pressurization fine purity, improving the purification rate of the 1, 4-cyclohexanedimethanol, and simultaneously detecting and knowing the peak time and the condition of the cis-trans isomer in the purified 1, 4-cyclohexanedimethanol so as to avoid the influence on the heat resistance of the product caused by the abnormal appearance of the cis-trans isomer in the purified 1, 4-cyclohexanedimethanol.

Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims

1. 1, 4-cyclohexanedimethanol purification device, including dissolution processing jar (1), its characterized in that: one side of dissolving treatment jar (1) is provided with PLC switch board (2), the top of dissolving treatment jar (1) communicates respectively has major ingredient charge door (3), ethylene glycol charge door (4) and acetone auxiliary agent charge door (5), the bottom of dissolving treatment jar (1) is through the material pipe intercommunication there is one-level material pump (6), one end that dissolving treatment jar (1) was kept away from to one-level material pump (6) is through the material pipe intercommunication there being decompression rectifying tank (7), there is second grade material pump (8) the bottom of decompression rectifying tank (7) is through the material pipe intercommunication, the one end that decompression rectifying tank (7) was kept away from to second grade material pump (8) is through the material pipe intercommunication there being pressure boost rectifying tank (9), the bottom intercommunication of pressure boost rectifying tank (9) has the fraction discharge gate, the inner chamber of dissolving treatment jar (1) is provided with aeration and removes miscellaneous mechanism (10), be provided with subregion temperature control mechanism (11) on dissolving treatment jar (1), decompression rectifying tank (7) and pressure boost rectifying tank (9) one side are provided with hydrogen feed mechanism (13) and pressure boost rectifying tank (9).

2. A 1, 4-cyclohexanedimethanol purification apparatus as in claim 1, wherein: the aeration impurity removing mechanism (10) comprises a primary filter (101), wherein the primary filter (101) is communicated with one side, close to a decompression rectifying tank (7), of a primary material pump (6), one side, close to a supercharging rectifying tank (9), of a secondary material pump (8) is communicated with a secondary filter (102), one side, fixedly connected with an aeration pump (103) at the top of a dissolution processing tank (1) and an air outlet of the aeration pump (103) are communicated with an aeration pipe (104), aeration holes (105) are formed in four ends of the aeration pipe (104), porous filter materials (106) are fixedly connected to the periphery of the inner wall of the dissolution processing tank (1), and filter holes (107) matched with the aeration holes (105) are formed in an inner cavity of the porous filter materials (106).

3. A 1, 4-cyclohexanedimethanol purification apparatus as in claim 1, wherein: the partition temperature control mechanism (11) comprises a first temperature sensor (111), one side of the bottom of the dissolution processing tank (1) is embedded with the first temperature sensor (111), the other side of the bottom of the dissolution processing tank (1) is embedded with a liquid sensor (112), the tops of the decompression rectifying tank (7) and the pressurization rectifying tank (9) are embedded with a second upper temperature sensor (113), the bottoms of the decompression rectifying tank (7) and the pressurization rectifying tank (9) are embedded with a second lower temperature sensor (114), one side of the dissolution processing tank (1), the decompression rectifying tank (7) and the pressurization rectifying tank (9) opposite to each other is provided with an electric heating box (115) and a first cable of the electric heating box (115) is provided with a first heating frame (116) which is covered with the dissolution processing tank (1), the inner cavities of the first heating frame (116) are fixedly connected with a first electric heating ring (117) which is matched with the dissolution processing tank (1), the bottoms of the electric heating box (115) and the second cable (1110) are provided with an auxiliary heating frame (118) which is covered with the second cable (119) respectively, the inner cavities of the two groups of the second upper heating frames (119) and the second lower heating frames (1110) are fixedly connected with second electric heating rings (1111) which are matched with the vacuum rectifying tank (7) and the pressurizing rectifying tank (9) for use.

4. A 1, 4-cyclohexanedimethanol purification apparatus as in claim 1, wherein: the utility model provides a hydrogen supply mechanism (12) is including hydrogen storage jar (121), hydrogen storage jar (121) set up in decompression rectifying tank (7) and one side that dissolution processing jar (1) was kept away from to pressure boost rectifying tank (9), the hydrogen outlet intercommunication of hydrogen storage jar (121) has pressure boost pump (122) and the hydrogen outlet intercommunication of pressure boost pump (122) has three way connection (123), the both ends of three way connection (123) all communicate branch pipe (124) and the other end intercommunication of branch pipe (124) have with decompression rectifying tank (7) and pressure boost rectifying tank (9) intercommunication complex buffer tube (125), two sets of buffer tube (125) are close to decompression rectifying tank (7) and pressure boost rectifying tank (9) one end is provided with pressure release valve (126).

5. A 1, 4-cyclohexanedimethanol purification apparatus as in claim 1, wherein: exhaust-gas treatment mechanism (13) are including exhaust-gas discharge pipe (131), exhaust-gas discharge pipe (131) intercommunication is at the top of dissolving processing jar (1), decompression rectifying tank (7) and pressure boost rectifying tank (9), exhaust-gas discharge pipe (131) are kept away from the top of dissolving processing jar (1), the one end intercommunication of decompression rectifying tank (7) and pressure boost rectifying tank (9) has processing case (132) and processing case (132) inner chamber from supreme active carbon adsorption layer (133) and filter membrane layer (134) of inlaying in proper order down, processing case (132) top joint has case lid (135), processing case (132) all offer heat dissipation window (136) near case lid (135) all around, the center department rotation of case lid (135) is connected with bull stick (137) and bull stick (137) top fixedly connected with fan (138), the bottom fixedly connected with of bull stick (137) and vortex (139) that heat dissipation window (136) cooperation was used.

6. A 1, 4-cyclohexanedimethanol purification apparatus as in claim 2, wherein: the aeration pipe (104) adopts spiral design, the aperture of aeration hole (105) is progressively reduced along the axis of aeration pipe (104) in proper order from top to bottom, porous filter material (106) is triangle equidistance state and adjacent contained angle is 120 along the axis of aeration pipe (104).

7. A 1, 4-cyclohexanedimethanol purification apparatus as in claim 3, wherein: the surfaces of the dissolution treatment tank (1), the decompression rectification tank (7) and the pressurization rectification tank (9) are respectively sleeved with a heat conduction pad (14) matched with the first electric heating ring (117) and the second electric heating ring (1111).

8. A 1, 4-cyclohexanedimethanol purification apparatus as in claim 5 wherein: the air guide fan (138) and the turbulent flow fan (139) are both in streamline design made of aluminum alloy materials, and the fan blades of the air guide fan (138) are larger than the fan blades of the turbulent flow fan (139) and are four.

9. A method for purifying 1, 4-cyclohexanedimethanol, a 1, 4-cyclohexanedimethanol purification apparatus according to any one of the preceding claims 1 to 8, characterized in that: the method comprises the following steps:

Step one: firstly, injecting a main material of the solid waxy 1, 4-cyclohexanedimethanol to be treated into a dissolution treatment tank (1) from a main material feed inlet (3), and then respectively injecting a glycol dissolver and an acetone auxiliary agent into the dissolution treatment tank (1) from a glycol feed inlet (4) and an acetone auxiliary agent feed inlet (5), wherein the molar ratio of the main material of the 1, 4-cyclohexanedimethanol, the glycol dissolver and the acetone auxiliary agent is 50:35:15, the PLC control cabinet (2) controls the electric heating box (115) to be started and the first electric heating ring (117) in the first heating frame (116) is electrified and heated through a first cable, the heat generated by the first electric heating ring (117) is conducted into the dissolution treatment tank (1) through the heat conduction pad (14), the solid waxy 1, 4-cyclohexanedimethanol main material in the dissolution treatment tank (1) is heated and dissolved, the temperature in the dissolution treatment tank (1) is detected by the first temperature sensor (111), the temperature in the dissolution treatment tank (1) is kept between 20 ℃ and 25 ℃, the liquid sensor (112) detects that the raw material in the dissolution treatment tank (1) is in a liquid state, meanwhile, the aeration pump (103) is controlled to be started, and high-pressure gas is applied into the aeration pipe (104), then the high-pressure gas is blown into the dissolution treatment tank (1) from top to bottom in a gradually decreasing state to form an aeration hole (105), the dissolved 1, 4-cyclohexanedimethanol main material, the ethylene glycol additive and the ethylene glycol additive are dissolved, the mixed solution is purified in the dissolution treatment tank (1) at the top of three-step-by step, the mixed solution is mixed with the mixed solution of the three-phase dissolution treatment tank (1) at the temperature of the top of the three-pressure and the three-phase filtration material (106) after the mixed solution is mixed with the clean solution in the dissolution tank (1), stopping the heating reaction to finish the preliminary dissolution of the 1, 4-cyclohexanedimethanol to obtain crude and pure products;

Step two: when the dissolution treatment tank (1) is heated to 20 ℃ and 25 ℃, a user correspondingly takes out a part of the crude and pure 1, 4-cyclohexanedimethanol solution which is preliminarily dissolved in the dissolution treatment tank (1) in the first step as a sample, and then carries out sample separation treatment on the molar ratio of the main material of the 1, 4-cyclohexanedimethanol, the glycol dissolvent and the auxiliary agent of the acetone in the crude and pure solution sample, and divides the sample into five component samples, wherein the molar ratio of the main material of the 1, 4-cyclohexanedimethanol, the glycol dissolvent and the auxiliary agent of the acetone in the five component samples is respectively 70:25: 5. 60:30: 10. 50:35: 15. 40:40:20 and 30:45:25, analysis 70 by gas chromatograph/mass spectrometer: 25: 5. 60:30: 10. 50:35: 15. 40:40:20 and 30:45:25 analyzing liquid phase, solid phase and dissolution phenomena of the 1, 4-cyclohexanedimethanol main material, the ethylene glycol dissolver and the acetone auxiliary agent in the crude pure solution sample at 20 ℃ and 25 ℃;

step three: then controlling a first-stage feed pump (6) to complete preliminary dissolution of crude 1, 4-cyclohexanedimethanol crude solution in a dissolution treatment tank (1) through a material pipe, filtering the crude solution by a first-stage filter (101), then feeding the crude solution into a pressure reduction rectification tank (7), controlling an electric heating box (115) to be opened by a PLC control cabinet (2) and electrifying a junction box (118) at the position of the pressure reduction rectification tank (7) through a second cable, synchronously generating heat by a second electric heating ring (1111) in a second upper heating frame (119) and a second lower heating frame (1110) which are distributed up and down in the pressure reduction rectification tank (7), correspondingly heating the top and the bottom of the pressure reduction rectification tank (7) through a heat conduction pad (14), simultaneously carrying out partition detection on the top and bottom temperatures of the pressure reduction rectification tank (7) by a second upper temperature sensor (113) and a second lower temperature sensor (114), keeping the top and bottom temperatures of the pressure reduction rectification tank (7) at 180 ℃ between 230 ℃ and 200 ℃ and the bottom temperatures, simultaneously opening a pressure reduction rectification valve (122) in the pressure reduction rectification tank (7) and a three-way pressure storage tank (122) at the pressure reduction rectification tank (7) at the same time, and opening a pressure reduction valve (122) in the pressure reduction rectification tank (7) at the pressure reduction rectification tank (7) and at the pressure of the pressure reduction tank (7) and the pressure reduction rectification tank (7), the hydrogen gas reaches the decompression rectifying tank (7) through the buffer tube (125), gas medium compensation is provided for the decompression rectifying reaction of the 1, 4-cyclohexanedimethanol crude pure solution until the tank top temperature and the tank bottom temperature of the decompression rectifying tank (7) reach the highest values at 210 ℃ and 230 ℃ correspondingly, and then the decompression fraction purifying work of the 1, 4-cyclohexanedimethanol crude pure solution in the decompression rectifying tank (7) is completed to obtain the 1, 4-cyclohexanedimethanol primary pure solution;

Step four: then the 1, 4-cyclohexane dimethanol primary rectification solution after the decompression distillation in the decompression rectification tank (7) is fed into the pressurization rectification tank (9) after being filtered by the secondary filter (102) through the secondary material pump (8), then the PLC control cabinet (2) controls the electric heating box (115) to be opened and is electrified to the junction box (118) at the position of the pressurization rectification tank (9) through the third cable, the second electric heating rings (1111) in the second upper heating frame (119) and the second lower heating frame (1110) are distributed up and down in the pressurization rectification tank (9), heat is synchronously generated correspondingly to the tank top and the tank bottom of the pressurization rectification tank (9) through the heat conduction pad (14), simultaneously, the second upper temperature sensor (113) and the second lower temperature sensor (114) on the pressurization rectification tank (9) are used for carrying out partition detection on the tank top and tank bottom temperature, the tank top temperature and the tank bottom temperature of the pressurization rectification tank (9) are kept between 200 ℃ and 220 ℃, the pressurization rectification tank top temperature and the tank bottom temperature are controlled to be kept between 200 ℃ and 220 ℃ and the pressure inside the three-way rectification tank (9) is controlled to be opened, the pressurization rectification tank (122) is opened and the pressurization rectification tank (9) is controlled to be opened by the three-way pressure valve (122) and the pressurization valve (122) is controlled to be opened in the pressurization rectification tank (1) (122) and the pressurization rectification tank (9), the hydrogen gas reaches the pressurizing rectifying tank (9) through the buffer tube (125), gas medium compensation is provided for pressurizing rectifying reaction of the 1, 4-cyclohexanedimethanol primary rectifying solution until the tank top temperature and the tank bottom temperature of the pressurizing rectifying tank (9) reach the highest values at 230 ℃ and 250 ℃ correspondingly, pressurizing fraction purifying work of the 1, 4-cyclohexanedimethanol primary rectifying solution in the pressurizing rectifying tank (9) is completed, 1, 4-cyclohexanedimethanol secondary rectifying solution is obtained, and finally the purified 1, 4-cyclohexanedimethanol secondary rectifying solution is discharged to the next working procedure section through a fraction discharge port of the pressurizing rectifying tank (9);

Step five: in the process of dissolving and purifying 1, 4-cyclohexanedimethanol main materials in turn in a dissolving treatment tank (1), a decompression rectifying tank (7) and a supercharging rectifying tank (9), the generated waste gas flows into a treatment tank (132) from three waste gas discharge pipes (131), then impurities such as metal particles and harmful substances in the waste gas generated in the dissolving treatment tank (1), the decompression rectifying tank (7) and the supercharging rectifying tank (9) are subjected to secondary filtration adsorption by an active carbon adsorption layer (133) and a filter membrane layer (134), natural wind force is captured by a guide fan (138) above a tank cover (135), and a rotating rod (137) is forced to drive a turbulent fan (139) to synchronously rotate along with the guide fan (138), so that the turbulent fan (139) rapidly discharges the waste gas purified gas subjected to secondary filtration from a radiating window (136) to the outside;