CN105348077A - Preparation method of p-phthaloyl chloride - Google Patents
Preparation method of p-phthaloyl chloride Download PDFInfo
- Publication number
- CN105348077A CN105348077A CN201510926724.3A CN201510926724A CN105348077A CN 105348077 A CN105348077 A CN 105348077A CN 201510926724 A CN201510926724 A CN 201510926724A CN 105348077 A CN105348077 A CN 105348077A
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- preparation
- tubular reactor
- phthaloyl chloride
- nitrogen
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/60—Preparation of carboxylic acid halides by conversion of carboxylic acids or their anhydrides or esters, lactones, salts into halides with the same carboxylic acid part
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/64—Separation; Purification; Stabilisation; Use of additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of p-phthaloyl chloride. The preparation method comprises the steps that terephthalic acid, a catalyst and thionyl chloride are added into a first tubular reactor for reaction, meanwhile, nitrogen is introduced into the first tubular reactor, the reacted materials successively enter into a first condenser and a first gas-liquid separator, vapor phases enter into an exhaust manifold, and liquid phases enter into a second tubular reactor; the nitrogen is introduced into the second tubular reactor, the materials successively enter into a second condenser and a second gas-liquid separator after removing a solvent, the vapor phases enter into the exhaust manifold, liquid-phase refining is performed to obtain the p-phthaloyl chloride. The preparation method of the p-phthaloyl chloride has the characteristics of being simple in process, continuous and efficient, the reaction period is greatly shortened, and the production efficiency is improved; the preparation method is conducive to mixing of reaction mass, rapidly bringing out the exhaust generated by reaction, improving the reaction rate, meanwhile, is conductive to removing the redundant solvent.
Description
Technical field
The invention belongs to chemosynthesis technical field, be specifically related to a kind of preparation method of p-phthaloyl chloride.
Background technology
P-phthaloyl chloride is important Organic Chemicals, is the raw material of the polymkeric substance such as polymeric amide, polyester, is the monomer of synthesis special fibre, can makes aramid fiber, polyamide fibre toughener.Aramid fiber is a kind of high-performance synthon, has superstrength, high temperature resistant, acid and alkali-resistance, the advantage such as lightweight, and toughness and intensity respectively can 2 times and 6 times of superior matter steel, in aircraft, rocket, guided missile and shellproof equipment.
Patent 201410517037.1 discloses a kind of continuous synthesis device of acyl chlorides and synthetic method, and it reacts in 730-750mmHg situation.
Summary of the invention
The object of this invention is to provide a kind of preparation method of p-phthaloyl chloride, there is simple, continuous, efficient feature, substantially reduce reaction time, improve production efficiency.
The preparation method of p-phthaloyl chloride of the present invention, step is as follows:
(1) terephthalic acid, catalyzer and sulfur oxychloride are joined in the first tubular reactor react, in the first tubular reactor, pass into nitrogen simultaneously, reacted material enters the first condenser, the first gas-liquid separator successively, gas phase enters engine manifold, and liquid phase enters the second tubular reactor;
(2) in the second tubular reactor, pass into nitrogen, enter the second condenser, the second gas-liquid separator after material desolvation successively, gas phase enters engine manifold, liquid-phase refining, to obtain final product.
Temperature of reaction described in step (1) is 70-100 DEG C.
Reaction pressure described in step (1) is-0.02-0.02Mpa.
The intake of the nitrogen described in step (1) is 50-500L/h.
The intake of the nitrogen described in step (2) is 5-200L/h.
The temperature of the desolvation described in step (2) is 90-130 DEG C, and vacuum tightness is not less than 650mmHg.
The present invention compared with prior art, has following beneficial effect:
The present invention has simple, continuous, the efficient feature of technique, substantially reduces reaction time, improves production efficiency; Be conducive to the mixing of reaction mass and be conducive to taking rapidly the tail gas reacting and produce out of, improving speed of reaction, be conducive to removing unnecessary solvent simultaneously.
Accompanying drawing explanation
Fig. 1 is the structural representation of present device;
In figure: 1, the first tubular reactor; 2, the first condenser; 3, the first gas-liquid separator; 4, the second tubular reactor; 5, the second condenser; 6, the second gas-liquid separator.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
(1) terephthalic acid, catalyzer and sulfur oxychloride are joined in the first tubular reactor react, temperature of reaction is 100 DEG C, reaction pressure is 0.02Mpa, in the first tubular reactor, pass into nitrogen simultaneously, the intake of nitrogen is 50-500L/h, reacted material enters the first condenser, the first gas-liquid separator successively, and gas phase enters engine manifold, and liquid phase enters the second tubular reactor;
(2) in the second tubular reactor, nitrogen is passed into, the intake of nitrogen is 5-200L/h, the second condenser, the second gas-liquid separator is entered successively after material desolvation, the temperature of desolvation is 130 DEG C, vacuum tightness is not less than 650mmHg, gas phase enters engine manifold, liquid-phase refining, to obtain final product.
Embodiment 2
(1) terephthalic acid, catalyzer and sulfur oxychloride are joined in the first tubular reactor react, temperature of reaction is 70 DEG C, reaction pressure is-0.02Mpa, in the first tubular reactor, pass into nitrogen simultaneously, the intake of nitrogen is 50-500L/h, reacted material enters the first condenser, the first gas-liquid separator successively, and gas phase enters engine manifold, and liquid phase enters the second tubular reactor;
(2) in the second tubular reactor, nitrogen is passed into, the intake of nitrogen is 5-200L/h, the second condenser, the second gas-liquid separator is entered successively after material desolvation, the temperature of desolvation is 90 DEG C, vacuum tightness is not less than 650mmHg, gas phase enters engine manifold, liquid-phase refining, to obtain final product.
Embodiment 3
(1) terephthalic acid, catalyzer and sulfur oxychloride are joined in the first tubular reactor react, temperature of reaction is 80 DEG C, reaction pressure is 0.01Mpa, in the first tubular reactor, pass into nitrogen simultaneously, the intake of nitrogen is 50-500L/h, reacted material enters the first condenser, the first gas-liquid separator successively, and gas phase enters engine manifold, and liquid phase enters the second tubular reactor;
(2) in the second tubular reactor, nitrogen is passed into, the intake of nitrogen is 5-200L/h, the second condenser, the second gas-liquid separator is entered successively after material desolvation, the temperature of desolvation is 120 DEG C, vacuum tightness is not less than 650mmHg, gas phase enters engine manifold, liquid-phase refining, to obtain final product.
Claims (6)
1. a preparation method for p-phthaloyl chloride, is characterized in that step is as follows:
(1) terephthalic acid, catalyzer and sulfur oxychloride are joined in the first tubular reactor react, in the first tubular reactor, pass into nitrogen simultaneously, reacted material enters the first condenser, the first gas-liquid separator successively, gas phase enters engine manifold, and liquid phase enters the second tubular reactor;
(2) in the second tubular reactor, pass into nitrogen, enter the second condenser, the second gas-liquid separator after material desolvation successively, gas phase enters engine manifold, liquid-phase refining, to obtain final product.
2. the preparation method of p-phthaloyl chloride according to claim 1, is characterized in that the temperature of reaction described in step (1) is 70-100 DEG C.
3. the preparation method of p-phthaloyl chloride according to claim 1, is characterized in that the reaction pressure described in step (1) is for-0.02-0.02Mpa.
4. the preparation method of p-phthaloyl chloride according to claim 1, is characterized in that the intake of the nitrogen described in step (1) is 50-500L/h.
5. the preparation method of p-phthaloyl chloride according to claim 1, is characterized in that the intake of the nitrogen described in step (2) is 5-200L/h.
6. the preparation method of p-phthaloyl chloride according to claim 1, it is characterized in that the temperature of the desolvation described in step (2) is 90-130 DEG C, vacuum tightness is not less than 650mmHg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510926724.3A CN105348077A (en) | 2015-12-14 | 2015-12-14 | Preparation method of p-phthaloyl chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510926724.3A CN105348077A (en) | 2015-12-14 | 2015-12-14 | Preparation method of p-phthaloyl chloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105348077A true CN105348077A (en) | 2016-02-24 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510926724.3A Pending CN105348077A (en) | 2015-12-14 | 2015-12-14 | Preparation method of p-phthaloyl chloride |
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| Country | Link |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112473609A (en) * | 2020-10-22 | 2021-03-12 | 杭州燕麟科技有限公司 | Sectional tubular reaction device and preparation method of cyclic phosphonate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101560146A (en) * | 2009-04-08 | 2009-10-21 | 淄博达隆制药科技有限公司 | Preparation method of paraphthaloyl chloride with high purity |
| CN101935276A (en) * | 2010-08-20 | 2011-01-05 | 南化集团研究院 | Synthetic method of p-phthaloyl chloride |
| CN102225895A (en) * | 2011-04-22 | 2011-10-26 | 仪征华纳生物科技有限公司 | Preparation method of terephthaloyl chloride |
| CN104402709A (en) * | 2014-12-12 | 2015-03-11 | 山东凯盛新材料有限公司 | Production technology and production device of terephthalyl chloride |
-
2015
- 2015-12-14 CN CN201510926724.3A patent/CN105348077A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101560146A (en) * | 2009-04-08 | 2009-10-21 | 淄博达隆制药科技有限公司 | Preparation method of paraphthaloyl chloride with high purity |
| CN101935276A (en) * | 2010-08-20 | 2011-01-05 | 南化集团研究院 | Synthetic method of p-phthaloyl chloride |
| CN102225895A (en) * | 2011-04-22 | 2011-10-26 | 仪征华纳生物科技有限公司 | Preparation method of terephthaloyl chloride |
| CN104402709A (en) * | 2014-12-12 | 2015-03-11 | 山东凯盛新材料有限公司 | Production technology and production device of terephthalyl chloride |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112473609A (en) * | 2020-10-22 | 2021-03-12 | 杭州燕麟科技有限公司 | Sectional tubular reaction device and preparation method of cyclic phosphonate |
| CN112473609B (en) * | 2020-10-22 | 2022-04-01 | 杭州燕麟科技有限公司 | Sectional tubular reaction device and preparation method of cyclic phosphonate |
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Application publication date: 20160224 |
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