CN105348078A - Recover method of thionyl chloride in continuous preparation process of p-phthaloyl chloride - Google Patents
Recover method of thionyl chloride in continuous preparation process of p-phthaloyl chloride Download PDFInfo
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- CN105348078A CN105348078A CN201510926851.3A CN201510926851A CN105348078A CN 105348078 A CN105348078 A CN 105348078A CN 201510926851 A CN201510926851 A CN 201510926851A CN 105348078 A CN105348078 A CN 105348078A
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- sulfur oxychloride
- film evaporator
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- recovery method
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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
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- 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 recover method of thionyl chloride in a continuous preparation process of p-phthaloyl chloride. The recover method comprises the steps that terephthalic acid, thionyl chloride and a catalyst are added into a mixing tank for mixing; mixed materials enter into the top of a feed tank from the bottom of the mixing tank; the materials in the feed tank is pressed into the top of a reaction still A from the bottom of the feed tank; the materials at the bottom of the reaction still A enter into the top of a reaction still B; the materials at the bottom of the reaction still B enter into the top of a reaction still C; materials which are fully reacted in the reaction still C enter into the top of a film evaporator; thionyl chloride light components at the top of the film evaporator pass through a first condenser, is recycled back to the reaction still A, and the materials at the bottom of the film evaporator enter into a refining system; pressure between all equipment is successively reduced. The recover method provided by the invention has the characteristics of being simple in process, continuous and efficient, the reaction period is greatly shortened, and the production efficiency is improved; meanwhile, a recover system of the thionyl chloride is optimized, and the technological process is greatly simplified.
Description
Technical field
The invention belongs to chemosynthesis technical field, be specifically related to the recovery method of sulfur oxychloride in a kind of p-phthaloyl chloride continuous production process.
Background technology
P-phthaloyl chloride is important Organic Chemicals, is the raw material of the polymkeric substance such as polymeric amide, polyester.It is the monomer of synthesis special fibre, aramid fiber, polyamide fibre toughener can be made, aramid fiber is a kind of high-performance synthon, there is superstrength, high temperature resistant, acid and alkali-resistance, the advantage such as lightweight, toughness and intensity respectively can 2 times and 6 times of superior matter steel, in aircraft, rocket, guided missile and shellproof equipment.
Patent 201210540394.0 discloses the recovery purification process of sulfur oxychloride in the production of a kind of acyl chlorides.
Patent 201410517623.6 discloses recovery purification devices and the recovery method of sulfur oxychloride in the production of a kind of acyl chlorides.
Summary of the invention
The object of this invention is to provide the recovery method of sulfur oxychloride in a kind of p-phthaloyl chloride continuous production process, there is simple, continuous, the efficient feature of technique, substantially reduce reaction time, improve production efficiency.
In p-phthaloyl chloride continuous production process of the present invention, the recovery method of sulfur oxychloride is by terephthalic acid, sulfur oxychloride and catalyzer join in mixing tank and mix, mix complete material and enter charging stock tank top bottom mixing tank, in charging stock tank, material is from press-in reactor A top, bottom, reactor A bottoms material enters reactor B top, reactor B bottoms material enters reactor C top, the reactor C material that reacts completely enters thin-film evaporator top, thin-film evaporator top sulfur oxychloride light constituent returns reactor A through the first condenser recycled, thin-film evaporator bottoms material enters refining system, between each equipment, pressure reduces successively.
The pressure of described reactor A is 0.1-0.2MPa.
The temperature of described reactor A is 70-80 DEG C.
The pressure of described reactor B is 0-0.1MPa.
The temperature of described reactor B is 80-90 DEG C.
The pressure of described reactor C is-0.05-0MPa.
The temperature of described reactor C is 90-100 DEG C.
In described thin-film evaporator, vacuum tightness is not less than 700mmHg.
The temperature of described thin-film evaporator is 100-140 DEG C.
The tail gas overall control that each reactor produces is between 100-500L/h.
The transfer of material between each storage tank, reactor adopts the mode of pressure reduction to carry out.
Material residence time between each reactor is 3-5 hour, and the sulfur oxychloride steamed directly is recycled to reactor A, achieves the recycle of sulfur oxychloride.
The liquid level of each storage tank, reactor, temperature, pressure all control to adopt Automated condtrol.
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; Optimize sulfur oxychloride recycling system simultaneously, enormously simplify technical process.
Accompanying drawing explanation
Fig. 1 is the structural representation of present device;
In figure: 1, mixing tank; 2, charging stock tank; 3, reactor A; 4, reactor B; 5, reactor C; 6, thin-film evaporator; 7, the first condenser; 8, the second condenser; 9, the 3rd condenser; 10, the 4th condenser; 11, variable valve.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
Terephthalic acid, sulfur oxychloride and catalyzer are mixed at mixing tank, mix complete material and enter charging stock tank top bottom mixing tank, open the exhaust system valve on the second condenser, the 3rd condenser, the 4th condenser terminal valve and reactor A, B, C, control tail gas amount between 100 ~ 200L/h, control the second condenser, the 3rd condenser, the 4th condenser cooling water temperature out between-20 ~ 60 DEG C; Rely on differential pressure action that material in charging stock tank is pressed into reactor A top after variable valve from bottom, reactor A bottoms material enters reactor B top after variable valve, reactor B bottoms material enters reactor C top after variable valve, and the reactor C material that reacts completely enters thin-film evaporator top; Thin-film evaporator top sulfur oxychloride light constituent applies mechanically back reactor A through the first condenser Posterior circle; Thin-film evaporator bottoms material enters refining system; Rely on differential pressure action that material is pressed into next equipment between neighbouring device, between each equipment, pressure reduces successively.Control reactor A temperature 70 DEG C, reactor B temperature 80 DEG C, reactor C temperature is at 90 DEG C; Control reactor A pressure at 0.2MPa, reactor B pressure in 0.1MPa, reactor C pressure at 0MPa; Control thin film evaporation actuator temperature to control at 100 DEG C, vacuum tightness is not less than 700mmHg.
Embodiment 2
Terephthalic acid, sulfur oxychloride and catalyzer are mixed at mixing tank, mix complete material and enter charging stock tank top bottom mixing tank, open the exhaust system valve on the second condenser, the 3rd condenser, the 4th condenser terminal valve and reactor A, B, C, control tail gas amount between 100 ~ 300L/h, control the second condenser, the 3rd condenser, the 4th condenser cooling water temperature out between-20 ~ 60 DEG C; Rely on differential pressure action that material in charging stock tank is pressed into reactor A top after variable valve from bottom, reactor A bottoms material enters reactor B top after variable valve, reactor B bottoms material enters reactor C top after variable valve, and the reactor C material that reacts completely enters thin-film evaporator top; Thin-film evaporator top sulfur oxychloride light constituent applies mechanically back reactor A through the first condenser Posterior circle; Thin-film evaporator bottoms material enters refining system; Rely on differential pressure action that material is pressed into next equipment between neighbouring device, between each equipment, pressure reduces successively.Control reactor A temperature 75 DEG C, reactor B temperature 90 DEG C, reactor C temperature is at 95 DEG C; Control reactor A pressure at 0.15MPa, reactor B pressure in 0.05MPa, reactor C pressure at-0.03MPa; Control thin film evaporation actuator temperature to control at 120 DEG C, vacuum tightness is not less than 700mmHg.
Embodiment 3
Terephthalic acid, sulfur oxychloride and catalyzer are mixed at mixing tank, mix complete material and enter charging stock tank top bottom mixing tank, open the exhaust system valve on the second condenser, the 3rd condenser, the 4th condenser terminal valve and reactor A, B, C, control tail gas amount between 100 ~ 500L/h, control the second condenser, the 3rd condenser, the 4th condenser cooling water temperature out between-20 ~ 60 DEG C; Rely on differential pressure action that material in charging stock tank is pressed into reactor A top after variable valve from bottom, reactor A bottoms material enters reactor B top after variable valve, reactor B bottoms material enters reactor C top after variable valve, and the reactor C material that reacts completely enters thin-film evaporator top; Thin-film evaporator top sulfur oxychloride light constituent applies mechanically back reactor A through the first condenser Posterior circle; Thin-film evaporator bottoms material enters refining system; Rely on differential pressure action that material is pressed into next equipment between neighbouring device, between each equipment, pressure reduces successively.Control reactor A temperature 80 DEG C, reactor B temperature 85 DEG C, reactor C temperature is at 100 DEG C; Control reactor A pressure at 0.1MPa, reactor B pressure in 0MPa, reactor C pressure at-0.05MPa; Control thin film evaporation actuator temperature to control at 140 DEG C, vacuum tightness is not less than 700mmHg.
Claims (9)
1. the recovery method of sulfur oxychloride in a p-phthaloyl chloride continuous production process, it is characterized in that terephthalic acid, sulfur oxychloride and catalyzer join in mixing tank and mix, mix complete material and enter charging stock tank top bottom mixing tank, in charging stock tank, material is from press-in reactor A top, bottom, reactor A bottoms material enters reactor B top, reactor B bottoms material enters reactor C top, the reactor C material that reacts completely enters thin-film evaporator top, thin-film evaporator top sulfur oxychloride light constituent returns reactor A through the first condenser recycled, thin-film evaporator bottoms material enters refining system, between each equipment, pressure reduces successively.
2. the recovery method of sulfur oxychloride in p-phthaloyl chloride continuous production process according to claim 1, is characterized in that the pressure of described reactor A is 0.1-0.2MPa.
3. the recovery method of sulfur oxychloride in p-phthaloyl chloride continuous production process according to claim 1 and 2, is characterized in that the temperature of described reactor A is 70-80 DEG C.
4. the recovery method of sulfur oxychloride in p-phthaloyl chloride continuous production process according to claim 1, is characterized in that the pressure of described reactor B is 0-0.1MPa.
5. the recovery method of sulfur oxychloride in the p-phthaloyl chloride continuous production process according to claim 1 or 4, is characterized in that the temperature of described reactor B is 80-90 DEG C.
6. the recovery method of sulfur oxychloride in p-phthaloyl chloride continuous production process according to claim 1, is characterized in that the pressure of described reactor C is-0.05-0MPa.
7. the recovery method of sulfur oxychloride in the p-phthaloyl chloride continuous production process according to claim 1 or 6, is characterized in that the temperature of described reactor C is 90-100 DEG C.
8. the recovery method of sulfur oxychloride in p-phthaloyl chloride continuous production process according to claim 1, is characterized in that in described thin-film evaporator, vacuum tightness is not less than 700mmHg.
9. the recovery method of sulfur oxychloride in the p-phthaloyl chloride continuous production process according to claim 1 or 8, is characterized in that the temperature of described thin-film evaporator is 100-140 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510926851.3A CN105348078A (en) | 2015-12-14 | 2015-12-14 | Recover method of thionyl chloride in continuous preparation process of p-phthaloyl chloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510926851.3A CN105348078A (en) | 2015-12-14 | 2015-12-14 | Recover method of thionyl chloride in continuous preparation process of p-phthaloyl chloride |
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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 CN201510926851.3A patent/CN105348078A/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 |
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Application publication date: 20160224 |