CN104045828A - Polyphenylene sulfide production method - Google Patents
Polyphenylene sulfide production method Download PDFInfo
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- CN104045828A CN104045828A CN201410325255.5A CN201410325255A CN104045828A CN 104045828 A CN104045828 A CN 104045828A CN 201410325255 A CN201410325255 A CN 201410325255A CN 104045828 A CN104045828 A CN 104045828A
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- polyphenylene sulfide
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Abstract
The invention discloses a polyphenylene sulfide production method, which comprises the following active ingredients: water-containing sodium sulfide, p-dichlorobenzene, phase solvent, solvent, and auxiliaries, wherein the phase solvent adopts 2-dimethyl benzoyl isocyanate, and the auxiliaries adopt chlorinated polyethylene. The polyphenylene sulfide production method concretely comprises the following steps: firstly, drying and dewatering the water-containing sodium sulfide, phase solvent, solvent, and auxiliaries, wherein the dewatering time lasts 30-50min, and the temperature is at 150-175DEG C; adding the p-dichlorobenzene after drying and dewatering, filtering after filtering, adding washing liquor while filtering, and filtering and rying to obtain polyphenylene sulfide. Through the mode, the invention can provide a polyphenylene sulfide production method, which is simple in operation steps, and easy to realize, the purity of polyphenylene sulfide can be controlled to the greatest extent during reaction, more refuses cannot be generated during reaction, and thus the environment can be effectively protected.
Description
Technical field
The present invention relates to a kind of engineering plastics production method, particularly relate to a kind of polyphenylene sulfide production method.
Background technology
Polyphenylene sulfide (Polyphenylene Sulfide is called for short PPS) is a kind of special engineering plastics of excellent performance, and world market all increases the demand of PPS and order, and domestic market is whole dependence on import almost.At present, China PPS is in the industrialization stage.In the study on the synthesis of PPS, formed multiple synthetic method.But the polyphenylene sulfide purity that the method finding out is produced is not high.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of polyphenylene sulfide production method, and operation steps is simple, easily realizes, and in reaction, can farthest control the purity of polyphenylene sulfide, and reaction can not produce more rubbish, effectively protection of the environment yet.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of polyphenylene sulfide production method is provided, comprise following raw material: moisture sodium sulphite, santochlor, phase solvent, solvent, auxiliary agent, described compatilizer adopts 2-dimethyl benzoyl isocyanic ester, and described auxiliary agent adopts chlorinatedpolyethylene.
Concrete operation step is: first moisture sodium sulphite, phase solvent, auxiliary agent are carried out to drying and dehydrating, described dewatering time is 30 ~ 50min, temperature is 150 ~ 175 degrees Celsius, after drying and dehydrating, being added into santochlor synthesizes, reaction generated time is 20 ~ 30min, and temperature is 175 ~ 195 degrees Celsius, after reaction, filters, when filtering, add washing lotion, can obtain polyphenylene sulfide filtering and be dried.
In a preferred embodiment of the present invention, dehydration liquid in described dehydrating step and the filtered liquid in filtration step enter water separation column and rectifying tower after collection, described dehydration liquid and filtrate, after water separation column, are carried out emission treatment by waste water or entering rectifying tower recycles.
In a preferred embodiment of the present invention, described washing lotion is sodium phosphate.
In a preferred embodiment of the present invention, in described water separation column and rectifying tower, be vacuum.
In a preferred embodiment of the present invention, described solvent is N-Methyl pyrrolidone.
The invention has the beneficial effects as follows: operation steps is simple, easily realize, and in reaction, can farthest control the purity of polyphenylene sulfide, reaction can not produce more rubbish, effectively protection of the environment yet.
Embodiment
Below the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only a part of embodiment of the present invention, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, not making all other embodiment that obtain under creative work prerequisite, belong to the scope of protection of the invention.
The embodiment of the present invention provides following technical scheme.
In one embodiment, a kind of polyphenylene sulfide production method, comprises following raw material: moisture sodium sulphite, santochlor, phase solvent, solvent, auxiliary agent.Described compatilizer adopts 2-dimethyl benzoyl isocyanic ester, and described auxiliary agent adopts chlorinatedpolyethylene, and described solvent is N-Methyl pyrrolidone.
The purity of 2-dimethyl benzoyl isocyanic ester is 80 ~ 90%, and chlorinatedpolyethylene purity is 70 ~ 95%, and N-Methyl pyrrolidone purity is 80 ~ 95%.
Concrete operation step is: first moisture sodium sulphite, phase solvent, auxiliary agent are carried out to drying and dehydrating, described dewatering time is 30 ~ 50min, temperature is 150 ~ 175 degrees Celsius, after drying and dehydrating, being added into santochlor synthesizes, reaction generated time is 20 ~ 30min, and temperature is 175 ~ 195 degrees Celsius, after reaction, filters, when filtering, add washing lotion, can obtain polyphenylene sulfide filtering and be dried.
Dehydration liquid in described dehydrating step and the filtered liquid in filtration step enter water separation column and rectifying tower after collection, and described dehydration liquid and filtrate, after water separation column, are carried out emission treatment by waste water or entering rectifying tower recycles.
Described washing lotion is sodium phosphate or water, can clean polyphenylene sulfide, makes purity increase.
In described water separation column and rectifying tower, be vacuum.
In one embodiment, a kind of polyphenylene sulfide production method, comprises following raw material: moisture sodium sulphite, santochlor, phase solvent, solvent, auxiliary agent.Described compatilizer adopts 2-dimethyl benzoyl isocyanic ester, and described auxiliary agent adopts chlorinatedpolyethylene, and described solvent is N-Methyl pyrrolidone.
The purity of 2-dimethyl benzoyl isocyanic ester is 80%, and chlorinatedpolyethylene purity is 70%, and N-Methyl pyrrolidone purity is 80%.
Concrete operation step is: first moisture sodium sulphite, phase solvent, auxiliary agent are carried out to drying and dehydrating, described dewatering time is 30min, temperature is 150 degrees Celsius, after drying and dehydrating, being added into santochlor synthesizes, reaction generated time is 20min, and temperature is 175 degrees Celsius, after reaction, filters, when filtering, add washing lotion, can obtain polyphenylene sulfide filtering and be dried.
Dehydration liquid in described dehydrating step and the filtered liquid in filtration step enter water separation column and rectifying tower after collection, and described dehydration liquid and filtrate, after water separation column, are carried out emission treatment by waste water or entering rectifying tower recycles.
Described washing lotion is sodium phosphate or water, can clean polyphenylene sulfide, makes purity increase.
In described water separation column and rectifying tower, be vacuum.
In one embodiment, a kind of polyphenylene sulfide production method, comprises following raw material: moisture sodium sulphite, santochlor, phase solvent, solvent, auxiliary agent.Described compatilizer adopts 2-dimethyl benzoyl isocyanic ester, and described auxiliary agent adopts chlorinatedpolyethylene, and described solvent is N-Methyl pyrrolidone.
The purity of 2-dimethyl benzoyl isocyanic ester is 90%, and chlorinatedpolyethylene purity is 95%, and N-Methyl pyrrolidone purity is 95%.
Concrete operation step is: first moisture sodium sulphite, phase solvent, auxiliary agent are carried out to drying and dehydrating, described dewatering time is 50min, temperature is 175 degrees Celsius, after drying and dehydrating, being added into santochlor synthesizes, reaction generated time is 30min, and temperature is 195 degrees Celsius, after reaction, filters, when filtering, add washing lotion, can obtain polyphenylene sulfide filtering and be dried.
Dehydration liquid in described dehydrating step and the filtered liquid in filtration step enter water separation column and rectifying tower after collection, and described dehydration liquid and filtrate, after water separation column, are carried out emission treatment by waste water or entering rectifying tower recycles.
Described washing lotion is sodium phosphate or water, can clean polyphenylene sulfide, makes purity increase.
In described water separation column and rectifying tower, be vacuum.
In one embodiment, a kind of polyphenylene sulfide production method, comprises following raw material: moisture sodium sulphite, santochlor, phase solvent, solvent, auxiliary agent.Described compatilizer adopts 2-dimethyl benzoyl isocyanic ester, and described auxiliary agent adopts chlorinatedpolyethylene, and described solvent is N-Methyl pyrrolidone.
The purity of 2-dimethyl benzoyl isocyanic ester is 85%, and chlorinatedpolyethylene purity is 80, and N-Methyl pyrrolidone purity is 90%.
Concrete operation step is: first moisture sodium sulphite, phase solvent, auxiliary agent are carried out to drying and dehydrating, described dewatering time is 40min, temperature is 160 degrees Celsius, after drying and dehydrating, being added into santochlor synthesizes, reaction generated time is 25min, and temperature is 190 degrees Celsius, after reaction, filters, when filtering, add washing lotion, can obtain polyphenylene sulfide filtering and be dried.
Dehydration liquid in described dehydrating step and the filtered liquid in filtration step enter water separation column and rectifying tower after collection, and described dehydration liquid and filtrate, after water separation column, are carried out emission treatment by waste water or entering rectifying tower recycles.
Described washing lotion is sodium phosphate or water, can clean polyphenylene sulfide, makes purity increase.
In described water separation column and rectifying tower, be vacuum.
The beneficial effect of polyphenylene sulfide production method of the present invention is: operation steps is simple, easily realizes, and in reaction, can farthest control the purity of polyphenylene sulfide, and reaction can not produce more rubbish, effectively protection of the environment yet.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes description of the present invention to do; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (5)
1. polyphenylene sulfide production formula and a method, is characterized in that, comprises following raw material: moisture sodium sulphite, santochlor, phase solvent, solvent, auxiliary agent, and described compatilizer adopts 2-dimethyl benzoyl isocyanic ester, and described auxiliary agent adopts chlorinatedpolyethylene; First moisture sodium sulphite, phase solvent, auxiliary agent are carried out to drying and dehydrating, described dewatering time is 30 ~ 50min, temperature is 150 ~ 175 degrees Celsius, after drying and dehydrating, being added into santochlor synthesizes, reaction generated time is about 20 ~ 30min, and temperature is 175 ~ 195 degrees Celsius, after reaction, filters, when filtering, add washing lotion, can obtain polyphenylene sulfide filtering and be dried.
2. a kind of polyphenylene sulfide production formula according to claim 1 and method, it is characterized in that, dehydration liquid in described dehydrating step and the filtered liquid in filtration step enter water separation column and rectifying tower after collection, described dehydration liquid and filtrate, after water separation column, are carried out emission treatment by waste water or entering rectifying tower recycles.
3. a kind of polyphenylene sulfide production formula according to claim 2 and method, is characterized in that, described washing lotion is sodium phosphate.
4. a kind of polyphenylene sulfide production formula according to claim 1 and method, is characterized in that, in described water separation column and rectifying tower, is vacuum.
5. a kind of polyphenylene sulfide production formula according to claim 1 and method, is characterized in that, described solvent is N-Methyl pyrrolidone.
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| CN201410325255.5A CN104045828A (en) | 2014-07-10 | 2014-07-10 | Polyphenylene sulfide production method |
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| CN201410325255.5A CN104045828A (en) | 2014-07-10 | 2014-07-10 | Polyphenylene sulfide production method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106478481A (en) * | 2016-10-08 | 2017-03-08 | 南京大学 | Waste water ultra-pure separation and purification technique of methyl pyrrolidone containing N and paracide |
Citations (5)
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| CN102432879A (en) * | 2011-08-11 | 2012-05-02 | 深圳市宝力特科技有限公司 | Dewatering process of polyhydrated sodium sulfide in synthetic process of polyphenylene sulfide resin |
| CN102560718A (en) * | 2012-01-04 | 2012-07-11 | 四川华通特种工程塑料研究中心有限公司 | Preparation method of surface coating type anti-oxidation polyphenylene sulfide fiber |
| CN103242528A (en) * | 2013-04-22 | 2013-08-14 | 中国石油化工股份有限公司 | Method for synthesizing linear high molecular weight polyphenyl thioether |
| CN103305003A (en) * | 2013-07-11 | 2013-09-18 | 常熟市慧丰塑料制品有限公司 | Formula of modified polyphenylene sulfide plastic |
| CN103571191A (en) * | 2013-11-08 | 2014-02-12 | 苏州市双赢包装材料有限公司 | Formula of modified polyphenylene sulfide resin |
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2014
- 2014-07-10 CN CN201410325255.5A patent/CN104045828A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432879A (en) * | 2011-08-11 | 2012-05-02 | 深圳市宝力特科技有限公司 | Dewatering process of polyhydrated sodium sulfide in synthetic process of polyphenylene sulfide resin |
| CN102560718A (en) * | 2012-01-04 | 2012-07-11 | 四川华通特种工程塑料研究中心有限公司 | Preparation method of surface coating type anti-oxidation polyphenylene sulfide fiber |
| CN103242528A (en) * | 2013-04-22 | 2013-08-14 | 中国石油化工股份有限公司 | Method for synthesizing linear high molecular weight polyphenyl thioether |
| CN103305003A (en) * | 2013-07-11 | 2013-09-18 | 常熟市慧丰塑料制品有限公司 | Formula of modified polyphenylene sulfide plastic |
| CN103571191A (en) * | 2013-11-08 | 2014-02-12 | 苏州市双赢包装材料有限公司 | Formula of modified polyphenylene sulfide resin |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106478481A (en) * | 2016-10-08 | 2017-03-08 | 南京大学 | Waste water ultra-pure separation and purification technique of methyl pyrrolidone containing N and paracide |
| CN106478481B (en) * | 2016-10-08 | 2018-07-06 | 南京大学 | The ultra-pure separation and purification technique of waste water containing N-Methyl pyrrolidone and paracide |
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Application publication date: 20140917 |