CN1312306A - Polyhydrated sodium sulfide dewatering techn during production of polyphenyl thioether - Google Patents
Polyhydrated sodium sulfide dewatering techn during production of polyphenyl thioether Download PDFInfo
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- CN1312306A CN1312306A CN00116141A CN00116141A CN1312306A CN 1312306 A CN1312306 A CN 1312306A CN 00116141 A CN00116141 A CN 00116141A CN 00116141 A CN00116141 A CN 00116141A CN 1312306 A CN1312306 A CN 1312306A
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- sodium
- water cure
- sodium sulfide
- dehydration
- many water
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Abstract
The present invention adopts polyhydrate sodium sulfide and p-dichlorobenzene as raw material, and utilizes the processes of dehydrating sodium sulfide and polycondensation to produce polyphenylene sulfide (PPS) monomer. It is characterized by that in the course of dehydration of polyhydrate sodium sulfide the polyhydrate sodium sulfide and NMP solution are heated in reactor to produce azeotropism at 180-220 deg.C so as to make crystal water of polyhydrate sodium sulfide be carried out with vapour phase. Said invention has no need of special dehydration equipment, and the temp. rising for dehydration is identical to the temp. rising direction of next operation for adding p-dichlorobenzene to implement polycondensation reaction, so it can prevent extra energy consumption.
Description
The present invention relates to the polyphenylene sulphide production process method improvement.
Adopting alkali metalsulphide and santochlor is that raw material is in the technological process of explained hereafter polyphenylene sulfide monomers (PPS) such as sodium sulphite dehydration, polycondensation, because alkali metalsulphide often has the crystal water that need remove, need carry out dewatering before the polycondensation at the adding santochlor for this reason.And conventional method is to set up special dehydration facility to dewater, and this has increased construction investment and operation site space on the one hand, needs extra energy expenditure on the other hand.
Above shortcoming in view of prior art, the objective of the invention is to create the many water cure sodium dewatering in a kind of polyphenylene sulfide production, dehydration operation and subsequent production are carried out in same reaction vessel, make it to have construction investment province, relatively little, the reasonable utilization of energy in space, place, the advantage of the little and production operation aspect of energy consumption.
Purpose of the present invention makes and realizes by following method.
Adopting many water cure sodium and santochlor (P-DCB) is raw material, through sodium sulphite dehydration-low molecule oligomerisation-explained hereafter polyphenylene sulfide monomers (PPS) such as polymer polycondensation.In many water cure of raw material sodium water smoking, with many water cure sodium and NMP (N-Methyl pyrrolidone) azeotropic of in reactor, heating, temperature 180-220 ℃; The crystal water of many water cure sodium is taken out of with vapor phase.
Adopt method of the present invention, directly the dissolving power of water is heated in reactor with NMP, allow many water cure sodium and NMP azeotropic, the steam that has water and NMP reclaims nmp solution through condensation separation, like this, can not build special sodium sulphite dehydration facility on the one hand specially, simplify equipment, save site space; The dehydration intensification is consistent with the intensification direction that system enters to polycondensation on the other hand, has avoided extra energy wastage.
Embodiment 1
In 25 liters of reactors, add Na
2S.3H
2Each 4 kilograms of O and NMP, catalyzer LiCl1.2 kilogram is heated to 200 ℃, keeps this temperature, and the system azeotropic is about two hours, and steam intermittently effluxes condensation, separates NMP and returns raw material.Dehydrating effect is good, and the product P PS polymerization that subsequent reactions makes is smooth, and molecular-weight average reaches 6 * 10
4
Embodiment 2
In 25 liters of reactors, add Na
2S.9H
24 kilograms of 4.7 kilograms of O and NMP, 1.2 kilograms of catalyzer LiCl are heated to 220 ℃ and keep this temperature, and system azeotropic 5-6 hour, steam drain into condensation outside intermittence, separate NMP and return raw material.Dehydrating effect is good, and the product P PS polymerization that subsequent reactions makes is smooth, and molecular-weight average reaches 6 * 10
4
Embodiment 3
In 25 liters of reactors, add Na
2S.9H
24 kilograms of 4.7 kilograms of O and NMP, 1.2 kilograms of catalyzer LiCl, pressure is heated to 180 ℃, keeps this temperature, and system azeotropic 4-5 hour, steam drain into condensation outside intermittence, separate NMP and return raw material.Dehydrating effect is good, and the product P PS polymerization that subsequent reactions makes is smooth, and molecular-weight average reaches 6 * 10
4
Embodiment 4
In 25 liters of reactors, add Na
2S.3H
2Each 4 kilograms of O and NMP, catalyzer LiCl1.2 kilogram is heated to 220 ℃, keeps this temperature, and the system azeotropic is about 2 hours, and the continuous outer condensation that drains into of steam separates NMP and returns raw material.Dehydrating effect is good, and the product P PS polymerization that subsequent reactions makes is smooth, and molecular-weight average reaches 6 * 10
4
The experiment proved that, adopt dewatering of the present invention, many advantages are also arranged on the accessibility of production operation, material repeatedly need not be carried, in a reactor, just can finish the operation of dehydration and subsequent reactions, simplified operation, made things convenient for production.
In addition, because NMP toxicity is minimum, so dewatering of the present invention also is feasible aspect environmental protection.
In actual production, heating is decided on the crystal water number of concrete used sodium sulphite the azeotropic time, in general, for three water cure sodium, the azeotropic time of heating be 1.5-2.5 hour for well; For nine water cure sodium, the azeotropic time of heating is to be advisable in 4-6 hour.
Claims (4)
1. the many water cure sodium dehydration technique during polyphenylene sulfide is produced, adopting many water cure sodium and santochlor is that raw material is produced the polyphenylene sulfide monomer through processing steps such as sodium sulphite dehydration, polycondensations, it is characterized in that, in many water cure of raw material sodium water smoking, with many water cure sodium and the nmp solution azeotropic of in reactor, heating, temperature 180-220 ℃; The crystal water of many water cure sodium is taken out of with vapor phase.
2. the many water cure sodium dehydration technique in producing according to the described polyphenylene sulfide of claim 1 is characterized in that described vapor phase is isolated NMP after condensation, and with its return raw material of doing.
3. the many water cure sodium dehydration technique in producing according to the described polyphenylene sulfide of claim 1 is characterized in that for three water cure sodium, the azeotropic time of heating is 1.5-2.5 hour.
4. the many water cure sodium dehydration technique in producing according to the described polyphenylene sulfide of claim 1 is characterized in that for nine water cure sodium, the azeotropic time of heating is 4-6 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00116141A CN1312306A (en) | 2000-09-30 | 2000-09-30 | Polyhydrated sodium sulfide dewatering techn during production of polyphenyl thioether |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00116141A CN1312306A (en) | 2000-09-30 | 2000-09-30 | Polyhydrated sodium sulfide dewatering techn during production of polyphenyl thioether |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1312306A true CN1312306A (en) | 2001-09-12 |
Family
ID=4585561
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN00116141A Withdrawn CN1312306A (en) | 2000-09-30 | 2000-09-30 | Polyhydrated sodium sulfide dewatering techn during production of polyphenyl thioether |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1312306A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100360586C (en) * | 2003-07-24 | 2008-01-09 | 东丽株式会社 | Process for producing polyaryl ylene sulfoether |
| 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 |
| CN103241716A (en) * | 2013-04-22 | 2013-08-14 | 中国石油化工股份有限公司 | Heating control method for dehydrating crystallized sodium sulfide for synthesizing polyphenylene sulfide |
| CN104262623A (en) * | 2014-08-28 | 2015-01-07 | 天津普莱化工技术有限公司 | Reduced pressure rectification and dehydration technique of polyphenylene sulfide raw material (crystalline sodium sulfide) |
| CN108147372A (en) * | 2017-12-05 | 2018-06-12 | 宜宾天原集团股份有限公司 | The preparation method of vulcanized sodium reacting precursor in polyphenylene sulfide production |
| CN111548492A (en) * | 2020-06-16 | 2020-08-18 | 四川明道和化学新材料有限公司 | Polyphenylene sulfide and synthetic method thereof |
-
2000
- 2000-09-30 CN CN00116141A patent/CN1312306A/en not_active Withdrawn
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100360586C (en) * | 2003-07-24 | 2008-01-09 | 东丽株式会社 | Process for producing polyaryl ylene sulfoether |
| 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 |
| CN102432879B (en) * | 2011-08-11 | 2013-07-24 | 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 |
| CN103241716A (en) * | 2013-04-22 | 2013-08-14 | 中国石油化工股份有限公司 | Heating control method for dehydrating crystallized sodium sulfide for synthesizing polyphenylene sulfide |
| CN104262623A (en) * | 2014-08-28 | 2015-01-07 | 天津普莱化工技术有限公司 | Reduced pressure rectification and dehydration technique of polyphenylene sulfide raw material (crystalline sodium sulfide) |
| CN108147372A (en) * | 2017-12-05 | 2018-06-12 | 宜宾天原集团股份有限公司 | The preparation method of vulcanized sodium reacting precursor in polyphenylene sulfide production |
| CN111548492A (en) * | 2020-06-16 | 2020-08-18 | 四川明道和化学新材料有限公司 | Polyphenylene sulfide and synthetic method thereof |
| CN111548492B (en) * | 2020-06-16 | 2023-02-24 | 四川明道和化学新材料有限公司 | Polyphenylene sulfide and synthesis method thereof |
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