CN102701960A - Method and device for refining crude products of m-phthaloyl chloride - Google Patents

Method and device for refining crude products of m-phthaloyl chloride Download PDF

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CN102701960A
CN102701960A CN2012101635972A CN201210163597A CN102701960A CN 102701960 A CN102701960 A CN 102701960A CN 2012101635972 A CN2012101635972 A CN 2012101635972A CN 201210163597 A CN201210163597 A CN 201210163597A CN 102701960 A CN102701960 A CN 102701960A
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tower
light constituent
phthaloyl chloride
rectifying tower
chlorine products
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刘丽艳
李洪
夏芃力
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Tianjin University
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Tianjin University
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Abstract

The invention relates to a method and a device for refining crude products of m-phthaloyl chloride. The crude products are heated to evaporate light components. The light components with boiling points lower than that of m-phthaloyl chloride are separated from bulk solution through a gasification and transferred into a light components continuous distillation system from an evaporation unit to be refined to obtain a small amount of light components and m-phthaloyl chloride in the tower and the light component products at tower top, which meet the requirements of national standards. The liquid of m-phthaloyl chloride crude products without the light components is transferred into an m-phthaloyl chloride continuous distillation system from the evaporation unit to be refined to obtain m-phthaloyl chloride product with a purity of 99.96% and a yield of over 90% at tower top. With the adoption of the device, a continuous treatment process is realized and the problems of low productivities of a single set of batch or semi-batch refining device and serious environmental pollutions caused by unqualified products are solved.

Description

M-phthaloyl chloride crude product refining method and apparatus
Invention field
The present invention relates to a kind of m-phthaloyl chloride crude product refining method and device, especially relate to a kind of employing continuous rectificating technique and carry out m-phthaloyl chloride crude product refining process and device thereof.
Background technology
M-phthaloyl chloride is a kind of organic industry raw material of outbalance; Can be used as the monomer of polymeric amide, polyester, polyarylester, polyaramide, liquid crystal polymer, aramid fiber 1313 (Nomax) etc.; Can be used as the properties-correcting agent of superpolymer simultaneously, the midbody of agricultural chemicals, medicine industry.Along with polyarylester advances to industriallization, increasingly extensive output and the purity requirement to m-phthaloyl chloride that aromatic poly is used increases day by day.
Different according to reaction mechanism, the preparation method of m-phthaloyl chloride has from acid, also have from ester, but the difference on the preparation method mainly is a chlorizating agent; Mainly contain sulfur oxychloride method, phosphorus pentachloride method, α, α, α; α ', α ', α ';-chlordene-m-xylene loses several kinds of chlorine method, phosgenation, ester chlorination and sour chlorinations etc., and the m-phthaloyl chloride that the reaction back generates is low because of purity, and fusing point has only about 80 ℃; And problems such as the m-phthaloyl chloride refining step periodical operation in the actual production process causes chlorizating agent to discharge to environment, causes environmental pollution, and the worker laboring environment is abominable.All documents of publishing all lay particular emphasis on synthetic reaction process about the introduction of m-phthaloyl chloride; And the concrete Technology of m-phthaloyl chloride bullion continuous treating is not all mentioned; The present invention is intended to propose a kind of continuous rectificating technique technology and equipment that is applied to the m-phthaloyl chloride crude product refining, solves problems such as present m-phthaloyl chloride refinement treatment amount is little, product index is defective, environmental pollution is serious.
Summary of the invention
The object of the invention is to provide a kind of continuous rectificating technique technology and equipment that is applied to the m-phthaloyl chloride crude product refining, solves problems such as present m-phthaloyl chloride refinement treatment amount is little, product index is defective, environmental pollution is serious.
The present invention realizes through following technical scheme:
M-phthaloyl chloride crude product refining method according to the invention; Bullion carries out the light constituent evaporation operation through heating; The light constituent that boiling point in the bullion is lower than m-phthaloyl chloride is vaporized from main body solution and separates; Light constituent after the vaporization leaves evaporation element entering light constituent continuous rectification Tower System and makes with extra care, and cat head obtains quality and satisfies the light constituent product that GB requires, and the tower still is a small amount of light constituent and m-phthaloyl chloride etc.The m-phthaloyl chloride bullion liquid phase that removes light constituent is left evaporation element and is got into m-phthaloyl chloride continuous rectification system and carry out product purification, and it is 99.96% isophthaloyl chlorine products that cat head obtains purity, and the heavy constituent of tower still are collected the back and reclaimed.
A kind of m-phthaloyl chloride crude product refining device according to the invention comprises the parallelly connected rectifying tower of evaporation unit and two system, and evaporation unit is provided with material inlet.One is light constituent continuous treating Tower System in the two parallelly connected rectifying tower systems, is provided with the light constituent admission port, and system comprises heating unit and overhead condensation device at the bottom of light constituent rectifying tower, the tower; Another Tower System is an isophthaloyl product purification Tower System, is provided with m-phthaloyl chloride and heavy constituent admission port, and system comprises heating unit and overhead condensation device at the bottom of isophthaloyl chlorine products rectifying tower, the tower; 2~100 theoretical stages of light constituent rectifying tower number of theoretical plate; 2~100 theoretical stages of isophthaloyl chlorine products rectifying tower number of theoretical plate.
Device of the present invention is characterized in that 5~15 theoretical stages of light constituent rectifying tower number of theoretical plate; 5~15 theoretical stages of isophthaloyl chlorine products rectifying tower number of theoretical plate.
Device of the present invention, it is characterized in that tower at the bottom of heating unit can adopt the tower body inner heating device, also can adopt the outer heating unit of tower body, the overhead condensation device can adopt condensing works in the tower body, also can adopt tower body condensed exterior device.
M-phthaloyl chloride crude product refining method of the present invention is characterized in that working pressure is 0.0001~200kPa in said light constituent rectifying tower system and the m-phthaloyl chloride continuous rectification system.
M-phthaloyl chloride crude product refining method of the present invention is characterized in that working pressure 100kPa in the light constituent rectifying tower system, working pressure 1~20kPa in the m-phthaloyl chloride continuous rectification system.
Beneficial effect of the present invention is to propose a kind of Technology and device that is applied to the m-phthaloyl chloride crude product refining; Adopt continuous rectificating technique technology and equipment to improve the treatment capacity and the quality product of m-phthaloyl chloride bullion, reach m-phthaloyl chloride chromatogram detection level>99.96% yield through the m-phthaloyl chloride quality product after the processing of this process for purification and reach more than 90%; Realize continuous treating processes, solve problems such as list overlaps intermittently or semi-batch refining plant throughput is low, and the defective environmental pollution of quality product is serious.
Description of drawings
Fig. 1: embodiment 1 m-phthaloyl chloride process for refining schematic flow sheet;
Inner heating device structural representation at the bottom of condensation and the tower in Fig. 2: the embodiment 2 light constituent rectifying tower cats head;
Outer heating unit structural representation at the bottom of condensation and the tower in Fig. 3: the embodiment 3 light constituent rectifying tower cats head;
Inner heating device structural representation at the bottom of Fig. 4: embodiment 4 light constituent rectifying tower cat head condensed exterior and the tower;
Inner heating device structural representation at the bottom of condensation and the tower in Fig. 5: the embodiment 2 isophthaloyl chlorine products rectifying tower cats head;
Outer heating unit structural representation at the bottom of condensation and the tower in Fig. 6: the embodiment 3 isophthaloyl chlorine products rectifying tower cats head;
Inner heating device structural representation at the bottom of Fig. 7: embodiment 4 isophthaloyl chlorine products rectifying tower cat head condensed exterior and the tower;
Wherein, 1-m-phthaloyl chloride bullion raw material, the m-phthaloyl chloride bullion after the 2-heating, the 3-evaporation removes the m-phthaloyl chloride bullion behind the light constituent; The vapour phase that 4-m-phthaloyl chloride bullion is evaporated, the heavy constituent of 5-isophthaloyl chlorine products rectifying tower tower still, 6-isophthaloyl chlorine products; Heavy constituent at the bottom of the 7-light constituent rectifying Tata, raw material or catalyzer after 8-is refining, 9-evaporates heating unit; The 10-evaporation unit, 11-isophthaloyl chlorine products rectifying tower, heating unit at the bottom of the 12-isophthaloyl chlorine products rectifying tower tower; 13-isophthaloyl chlorine products rectifying tower overhead condensation device, 14-isophthaloyl chlorine products rectifying tower trim the top of column device, 15-light constituent rectifying tower; Heating unit at the bottom of the 16-light constituent rectifying Tata, 17-light constituent rectifying tower overhead condensation device, 18-light constituent rectifying tower trim the top of column device.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is explained further details:
Equipment connects as shown in Figure 1: m-phthaloyl chloride bullion raw material (1) is sent into evaporation unit (10) via heating unit (9); The vapour phase that the m-phthaloyl chloride bullion is evaporated (4) gets in the light constituent rectifying tower (15) carries out distillation operation; Heating unit (16) provides heat for the material vaporization at the bottom of the light constituent rectifying Tata; Steam after the vaporization rises to light constituent rectifying tower cat head and is condensed into liquid phase entering light constituent rectifying tower trim the top of column device (5) by overhead condensation device (17); Liquid phase part in the light constituent rectifying tower trim the top of column device refluxes and gets into the light constituent rectifying tower; By extraction, collect at the bottom of the light constituent rectifying Tata by heavy constituent (7) extraction at the bottom of the tower as the raw material after refining or catalyzer (8) for another part.Process evaporation unit (10) evaporation removes in m-phthaloyl chloride bullion (3) the entering isophthaloyl chlorine products rectifying tower (10) behind the light constituent carries out distillation operation.Isophthaloyl chlorine products rectifying tower tower still heating unit (14) provides heat for the material vaporization; Steam after the vaporization rises to isophthaloyl chlorine products rectifying tower cat head; Be condensed into liquid phase by isophthaloyl chlorine products rectifying tower overhead condensation device (13) and get into isophthaloyl chlorine products rectifying tower trim the top of column device (14); Liquid phase part in the isophthaloyl chlorine products rectifying tower trim the top of column device refluxes and gets into isophthaloyl chlorine products rectifying tower; Another part is as isophthaloyl chlorine products (6) extraction, and isophthaloyl chlorine products rectifying tower tower still heavy constituent (5) extraction at the bottom of the tower is collected.
Embodiment 1:
Description of equipment: heating unit (16) all adopts external structure as shown in Figure 1 at the bottom of light constituent rectifying tower overhead condensation device (17) and the light constituent rectifying Tata.Heating unit (12) also adopts external structure as shown in Figure 1 at the bottom of isophthaloyl chlorine products rectifying tower overhead condensation device (13) and the isophthaloyl chlorine products rectifying tower tower.
M-phthaloyl chloride bullion raw material (1) is formed as follows: m-phthaloyl chloride 70%, sulfur oxychloride 26%, DMF1%, other light constituent (boiling point is lower than m-phthaloyl chloride) 0.5%, heavy constituent (boiling point is higher than m-phthaloyl chloride) 2.5%.As shown in Figure 1, m-phthaloyl chloride bullion raw material (1) is sent in the evaporation unit (10) via heating unit (9) and is evaporated light constituent raw material or catalyzer, mainly is sulfur oxychloride and DMF in the present embodiment, evaporation unit internal pressure 100kPa.The light constituent that is evaporated (4) gets in the light constituent rectifying tower (15) and carries out distillation operation; 10 theoretical stages of light constituent rectifying tower; Working pressure 100kPa (absolute pressure) in the tower; Heating unit (16) provides heat for the material vaporization at the bottom of the light constituent rectifying Tata; Steam after the vaporization rises to light constituent rectifying tower cat head and is condensed into liquid phase entering light constituent rectifying tower trim the top of column device (5) by overhead condensation device (17), and the liquid phase part in the light constituent rectifying tower trim the top of column device refluxes and gets into the light constituent rectifying tower, and raw material after another part conduct is made with extra care or catalyzer (8) are by extraction; Product purity can reach the GB requirement, and heavy constituent (7) extraction at the bottom of the tower is collected at the bottom of the light constituent rectifying Tata.Process evaporation unit (10) evaporation removes in m-phthaloyl chloride bullion (3) the entering isophthaloyl chlorine products rectifying tower (10) behind the light constituent carries out distillation operation.10 theoretical stages of isophthaloyl chlorine products rectifying tower; Working pressure 0.001kPa (absolute pressure) in the tower; Isophthaloyl chlorine products rectifying tower tower still heating unit (14) provides heat for the material vaporization; Steam after the vaporization rises to isophthaloyl chlorine products rectifying tower cat head, is condensed into liquid phase by isophthaloyl chlorine products rectifying tower overhead condensation device (13) and gets into isophthaloyl chlorine products rectifying tower trim the top of column device (14), and the liquid phase part in the isophthaloyl chlorine products rectifying tower trim the top of column device refluxes and gets into isophthaloyl chlorine products rectifying tower; Another part is as isophthaloyl chlorine products (6) extraction; Quality reaches m-phthaloyl chloride chromatogram detection level>99.96%, and yield reaches 92%, and isophthaloyl chlorine products rectifying tower tower still heavy constituent (5) extraction at the bottom of the tower is collected.Equipment size can be adjusted according to the size of treatment capacity in the complete assembly, and it is low to solve single cover intermittence or semi-batch refining plant throughput, the underproof problem of quality product.All materials are continuous airtight operation in system, materials such as chlorizating agent can not occur and discharge to environment, causes problems such as environmental pollution and worker laboring environment deterioration.
Embodiment 2:
Description of equipment: heating unit (16) all adopts embedding structure as shown in Figure 2 at the bottom of light constituent rectifying tower overhead condensation device (17) and the light constituent rectifying Tata.Heating unit (12) adopts embedding structure as shown in Figure 5 at the bottom of isophthaloyl chlorine products rectifying tower overhead condensation device (13) and the isophthaloyl chlorine products rectifying tower tower.
M-phthaloyl chloride bullion raw material (1) is formed as follows: m-phthaloyl chloride 65%, sulfur oxychloride 28%, pyridine 3%, other light constituent (boiling point is lower than m-phthaloyl chloride) 1.5%, heavy constituent (boiling point is higher than m-phthaloyl chloride) 2.5%.As shown in Figure 1, m-phthaloyl chloride bullion raw material (1) is sent in the evaporation unit (10) via heating unit (9) and is evaporated light constituent raw material or catalyzer, mainly is sulfur oxychloride and pyridine in the present embodiment, evaporation unit internal pressure 120kPa.The light constituent that is evaporated (4) gets in the light constituent rectifying tower (15) and carries out distillation operation; 15 theoretical stages of light constituent rectifying tower; Working pressure 120kPa (absolute pressure) in the tower; Heating unit (16) provides heat for the material vaporization at the bottom of the light constituent rectifying Tata; Steam after the vaporization rises to light constituent rectifying tower cat head and is condensed into liquid phase entering light constituent rectifying tower trim the top of column device (5) by light constituent rectifying tower overhead condensation device (17), and the liquid phase part in the light constituent rectifying tower trim the top of column device refluxes and gets into the light constituent rectifying tower, and raw material after another part conduct is made with extra care or catalyzer (8) are by extraction; Product purity can reach the GB requirement, and heavy constituent (7) extraction at the bottom of the tower is collected at the bottom of the light constituent rectifying Tata.Process evaporation unit (10) evaporation removes in m-phthaloyl chloride bullion (3) the entering isophthaloyl chlorine products rectifying tower (10) behind the light constituent carries out distillation operation.15 theoretical stages of m-phthaloyl chloride product purification tower; Working pressure 0.01kPa (absolute pressure) in the tower; Isophthaloyl chlorine products rectifying tower tower still heating unit (14) provides heat for the material vaporization; Steam after the vaporization rises to isophthaloyl chlorine products rectifying tower cat head, is condensed into liquid phase by isophthaloyl chlorine products rectifying tower overhead condensation device (13) and gets into isophthaloyl chlorine products rectifying tower trim the top of column device (14), and the liquid phase part in the isophthaloyl chlorine products rectifying tower trim the top of column device refluxes and gets into isophthaloyl chlorine products rectifying tower; Another part is as isophthaloyl chlorine products (6) extraction; Quality reaches m-phthaloyl chloride chromatogram detection level>99.96%, and yield reaches 91%, and isophthaloyl chlorine products rectifying tower tower still heavy constituent (5) extraction at the bottom of the tower is collected.Equipment size can be adjusted according to the size of treatment capacity in the complete assembly, and it is low to solve single cover intermittence or semi-batch refining plant throughput, the underproof problem of quality product.All materials are continuous airtight operation in system, materials such as chlorizating agent can not occur and discharge to environment, causes problems such as environmental pollution and worker laboring environment deterioration.
Embodiment 3:
Description of equipment:
Heating unit (16) adopted external structure at the bottom of light constituent rectifying tower overhead condensation device (17) adopted embedding structure and light constituent rectifying Tata, and is as shown in Figure 3.Heating unit (12) adopted external structure as shown in Figure 6 at the bottom of isophthaloyl chlorine products rectifying tower overhead condensation device (13) adopted embedding structure and isophthaloyl chlorine products rectifying tower tower.
M-phthaloyl chloride bullion raw material (1) is formed as follows: m-phthaloyl chloride 72%, TRIPHOSGENE 99.5 26%, DMF1%, other light constituent (boiling point is lower than m-phthaloyl chloride) 0.5%, heavy constituent (boiling point is higher than m-phthaloyl chloride) 0.5%.As shown in Figure 1, m-phthaloyl chloride bullion raw material (1) is sent in the evaporation unit (10) via heating unit (9) and is evaporated light constituent raw material or catalyzer, mainly is TRIPHOSGENE 99.5 and DMF in the present embodiment, evaporation unit internal pressure 150kPa.The light constituent that is evaporated (4) gets in the light constituent rectifying tower (15) and carries out distillation operation; 5 theoretical stages of light constituent rectifying tower; Working pressure 200kPa (absolute pressure) in the tower; Heating unit (16) provides heat for the material vaporization at the bottom of the light constituent rectifying Tata; Steam after the vaporization rises to light constituent rectifying tower cat head and is condensed into liquid phase entering light constituent rectifying tower trim the top of column device (5) by light constituent rectifying tower overhead condensation device (17), and the liquid phase part in the light constituent rectifying tower trim the top of column device refluxes and gets into the light constituent rectifying tower, and raw material after another part conduct is made with extra care or catalyzer (8) are by extraction; Product purity can reach the GB requirement, and heavy constituent (7) extraction at the bottom of the tower is collected at the bottom of the light constituent rectifying Tata.Process evaporation unit (10) evaporation removes in m-phthaloyl chloride bullion (3) the entering isophthaloyl chlorine products rectifying tower (10) behind the light constituent carries out distillation operation.5 theoretical stages of isophthaloyl chlorine products rectifying tower; Working pressure 20kPa (absolute pressure) in the tower; Heating unit (14) provides heat for the material vaporization at the bottom of the isophthaloyl chlorine products rectifying tower tower; Steam after the vaporization rises to isophthaloyl chlorine products rectifying tower cat head, is condensed into liquid phase by isophthaloyl chlorine products rectifying tower overhead condensation device (13) and gets into isophthaloyl chlorine products rectifying tower trim the top of column device (14), and the liquid phase part in the isophthaloyl chlorine products rectifying tower trim the top of column device refluxes and gets into isophthaloyl chlorine products rectifying tower; Another part is as isophthaloyl chlorine products (6) extraction; Quality reaches m-phthaloyl chloride chromatogram detection level>99.96%, and yield reaches 90%, and isophthaloyl chlorine products rectifying tower tower still heavy constituent (5) extraction at the bottom of the tower is collected.Equipment size can be adjusted according to the size of treatment capacity in the complete assembly, and it is low to solve single cover intermittence or semi-batch refining plant throughput, the underproof problem of quality product.All materials are continuous airtight operation in system, materials such as chlorizating agent can not occur and discharge to environment, causes problems such as environmental pollution and worker laboring environment deterioration.
Embodiment 4:
Description of equipment: heating unit (16) adopted embedding structure at the bottom of light constituent rectifying tower overhead condensation device (17) adopted external structure and light constituent rectifying Tata, and is as shown in Figure 4.Heating unit (12) adopted embedding structure as shown in Figure 7 at the bottom of isophthaloyl chlorine products rectifying tower overhead condensation device (13) adopted external structure and isophthaloyl chlorine products rectifying tower tower.
M-phthaloyl chloride bullion raw material (1) is formed as follows: m-phthaloyl chloride 75%, POCl3 23%, other light constituent (boiling point is lower than m-phthaloyl chloride) 0.5%, heavy constituent (boiling point is higher than m-phthaloyl chloride) 1.5%.As shown in Figure 1, m-phthaloyl chloride bullion raw material (1) is sent in the evaporation unit (10) via heating unit (9) and is evaporated light constituent raw material or catalyzer, mainly is POCl3 in the present embodiment, evaporation unit internal pressure 90kPa.The light constituent that is evaporated (4) gets in the light constituent rectifying tower (15) and carries out distillation operation; 20 theoretical stages of light constituent rectifying tower; Working pressure 90kPa (absolute pressure) in the tower; Heating unit (16) provides heat for the material vaporization at the bottom of the light constituent rectifying Tata; Steam after the vaporization rises to light constituent rectifying tower cat head and is condensed into liquid phase entering light constituent rectifying tower trim the top of column device (5) by light constituent rectifying tower overhead condensation device (17), and the liquid phase part in the light constituent rectifying tower trim the top of column device refluxes and gets into the light constituent rectifying tower, and raw material after another part conduct is made with extra care or catalyzer (8) are by extraction; Product purity can reach the GB requirement, and heavy constituent (7) extraction at the bottom of the tower is collected at the bottom of the light constituent rectifying Tata.Process evaporation unit (10) evaporation removes in m-phthaloyl chloride bullion (3) the entering m-phthaloyl chloride treating tower (heavy tower) (10) behind the light constituent carries out distillation operation.20 theoretical stages of isophthaloyl chlorine products rectifying tower; Working pressure 1kPa (absolute pressure) in the tower; Isophthaloyl chlorine products rectifying tower tower still heating unit (14) provides heat for the material vaporization; Steam after the vaporization rises to isophthaloyl chlorine products rectifying tower cat head, is condensed into liquid phase by isophthaloyl chlorine products rectifying tower overhead condensation device (13) and gets into isophthaloyl chlorine products rectifying tower trim the top of column device (14), and the liquid phase part in the isophthaloyl chlorine products rectifying tower trim the top of column device refluxes and gets into isophthaloyl chlorine products rectifying tower; Another part is as isophthaloyl chlorine products (6) extraction; Quality reaches m-phthaloyl chloride chromatogram detection level>99.96%, and yield reaches 95%, and isophthaloyl chlorine products rectifying tower tower still heavy constituent (5) extraction at the bottom of the tower is collected.Equipment size can be adjusted according to the size of treatment capacity in the complete assembly, and it is low to solve single cover intermittence or semi-batch refining plant throughput, the underproof problem of quality product.All materials are continuous airtight operation in system, materials such as chlorizating agent can not occur and discharge to environment, causes problems such as environmental pollution and worker laboring environment deterioration.
M-phthaloyl chloride continuous refining process technology and equipment that the present invention proposes are described through preferred embodiment; Person skilled obviously can be in not breaking away from content of the present invention, spirit and scope to structure as herein described with equipment is changed or suitably change and combination, realize the present invention's technology.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as and are included in spirit of the present invention, scope and the content.

Claims (6)

1. m-phthaloyl chloride crude product refining method; It is characterized in that bullion carries out the light constituent evaporation operation through heating; The light constituent that boiling point in the bullion is lower than m-phthaloyl chloride is vaporized from main body solution and separates; Light constituent after the vaporization leaves evaporation element entering light constituent continuous rectification Tower System and makes with extra care, and cat head obtains quality and satisfies the light constituent product that GB requires, and the tower still is a small amount of light constituent and m-phthaloyl chloride etc.; The m-phthaloyl chloride bullion liquid phase that removes light constituent is left evaporation element and is got into m-phthaloyl chloride continuous rectification system and carry out product purification, and it is 99.96% isophthaloyl chlorine products that cat head obtains purity, and the heavy constituent of tower still are collected the back and reclaimed.
2. m-phthaloyl chloride crude product refining device is characterized in that comprising the parallelly connected rectifying tower of evaporation unit and two system, and evaporation unit is provided with material inlet; One is light constituent continuous treating Tower System in the two parallelly connected rectifying tower systems, is provided with the light constituent admission port, and system comprises heating unit and overhead condensation device at the bottom of light constituent rectifying tower, the tower; Another rectifying tower system is an isophthaloyl product purification Tower System, is provided with m-phthaloyl chloride and heavy constituent admission port, and system comprises heating unit and overhead condensation device at the bottom of isophthaloyl chlorine products rectifying tower, the tower; 2~100 theoretical stages of light constituent rectifying tower number of theoretical plate; 2~100 theoretical stages of isophthaloyl chlorine products rectifying tower number of theoretical plate.
3. device as claimed in claim 2 is characterized in that 5~15 theoretical stages of light constituent rectifying tower number of theoretical plate; 5~15 theoretical stages of isophthaloyl chlorine products rectifying tower number of theoretical plate.
4. device as claimed in claim 2 is characterized in that heating unit adopts the tower body inner heating device at the bottom of the tower, or adopts the outer heating unit of tower body, and the overhead condensation device adopts condensing works in the tower body, or adopts tower body condensed exterior device.
5. the method for claim 1 is characterized in that working pressure is 0.0001~200kPa in said light constituent rectifying tower system and the m-phthaloyl chloride continuous rectification system.
6. the method for claim 1 is characterized in that working pressure 100kPa in the light constituent rectifying tower system, working pressure 1~20kPa in the m-phthaloyl chloride continuous rectification system.
CN2012101635972A 2012-05-22 2012-05-22 Method and device for refining crude products of m-phthaloyl chloride Pending CN102701960A (en)

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CN104261355A (en) * 2014-09-30 2015-01-07 烟台裕祥精细化工有限公司 Recovering and purifying device and recovering method of thionyl chloride in acyl chloride production
CN104262084A (en) * 2014-09-12 2015-01-07 上海方纶新材料科技有限公司 Process and device for continuous rectification of bis(trichloromethyl)benzene
CN104744232A (en) * 2015-03-18 2015-07-01 湖南海利常德农药化工有限公司 Method for preparing isophthaloyl dichloride
CN105126374A (en) * 2015-06-29 2015-12-09 天津市天地创智科技发展有限公司 tert-Butanol-water-cyclohexanone oxime differential-pressure rectification system
CN109336759A (en) * 2018-12-03 2019-02-15 山东民基化工有限公司 Continuously prepare the method and device thereof of chloro-pivalyl chloride
CN110872216A (en) * 2019-12-06 2020-03-10 南京恒道医药科技有限公司 Method and device for producing (2-chloro-5-iodophenyl) -4-fluorobenzyl ketone by reaction separation coupling
CN111643918A (en) * 2020-06-16 2020-09-11 山东中盛药化设备有限公司 Rectification purification device and purification method for multi-component material

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Publication number Priority date Publication date Assignee Title
CN104262084A (en) * 2014-09-12 2015-01-07 上海方纶新材料科技有限公司 Process and device for continuous rectification of bis(trichloromethyl)benzene
CN104225946A (en) * 2014-09-30 2014-12-24 烟台裕祥精细化工有限公司 Continuous rectifying device and rectifying method for acyl chloride
CN104261355A (en) * 2014-09-30 2015-01-07 烟台裕祥精细化工有限公司 Recovering and purifying device and recovering method of thionyl chloride in acyl chloride production
CN104225946B (en) * 2014-09-30 2016-08-17 烟台裕祥精细化工有限公司 The continuous rectification apparatus of a kind of acyl chlorides and rectificating method
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Application publication date: 20121003