CN85109096B - Synthelization of linear macromolecular polybenzewne thioether - Google Patents
Synthelization of linear macromolecular polybenzewne thioether Download PDFInfo
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- CN85109096B CN85109096B CN85109096A CN85109096A CN85109096B CN 85109096 B CN85109096 B CN 85109096B CN 85109096 A CN85109096 A CN 85109096A CN 85109096 A CN85109096 A CN 85109096A CN 85109096 B CN85109096 B CN 85109096B
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- hydrogen sulphide
- hydrogen sulfide
- waste gas
- raw materials
- sodium phosphate
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Abstract
The present invention relates to a method for obtaining high molecular weight linear polyphenylene sulfide by using hydrogen sulphide and p-dichlorobenzene as raw materials, hexamethylphosphamide as a solvent and sodium phosphate as an auxiliary agent in the presence of a third component through polymerization at normal pressure. The present invention has the characteristics of wide hydrogen sulphide sources, low hydrogen sulphide price, simple required equipment, short reaction period, high product yield, high product quality, low production cost, waste gas utilization, change of wastes into valuables, conversion of harm into benefit, and obvious economic benefits. Hydrogen sulphide, such as natural gas desulfurized sour gas and carbon disulfide produced hydrogen sulphide as waste gas, as waste gas in a factory can be used as one of the raw materials in the method, and hydrogen sulphide, etc. generated by sulfur iron ore can also be used as one of the raw materials in the method. The method is an effective method for protecting the environment. C08K3: 10).
Description
The invention belongs to the improvement of the synthetic method of linear polyphenylthioether of high molecular weight (hereinafter to be referred as HMWPPS).
The method of general synthesized polymer thioether, as United States Patent (USP) 4,373,090 is described, with hydrogen sulfide, santochlor and sodium hydroxide is raw material, make auxiliary agent with sodium acetate, anhydrous (or yellow soda ash), wherein sodium acetate, anhydrous (or yellow soda ash) is 0.5: 1.0 with the mol amount ratio of hydrogen sulfide, adds 15-18kg/cm at 204-266 ℃
2Carried out polyreaction 5-8 hour in the N-N-methyl-2-2-pyrrolidone N-solvent of pressure, the melting index that obtains polyphenylene sulfide is 6150-454(ASTMD1238-70,316 ℃, and 5kg, gram/10 minute).The weak point of this method is reaction pressurization, equipment complexity, and the time is longer, and molecular weight of product is low, the aftertreatment difficulty, and cost is higher.
The objective of the invention is to overcome the deficiency of prior art, and make one of raw material with waste gas hydrogen sulfide in hydrogen sulfide, the especially factory, find a suitable approach, synthetic HMWPPS is in order to industrial production.
Main points of the present invention are to be raw material with hydrogen sulfide, santochlor and sodium hydroxide, its hydrogen sulfide can be waste gas hydrogen sulfide in the factory, as the acid gas of selexol process, the hydrogen sulfide producing the waste gas etc. of dithiocarbonic anhydride, also can take place with sulfurous iron ore, wherein (contain H with the waste gas of producing dithiocarbonic anhydride
2S94%, H
23.54%, CS
21.78%, CH
41%) for well.Add anhydrous sodium phosphate and make auxiliary agent, its mol amount ratio is a santochlor: hydrogen sulfide: sodium hydroxide: anhydrous sodium phosphate=1～1.02: 1: 2: 0.5-2.20.Make solvent with hempa, carry out polymerization under atmospheric pressure reaction 3-4 hour at 180-235 ℃, obtain HMWPPS through separation, output is more than 95%, and melt viscosity reaches 7 * 10
4Pool (303 ℃ of mensuration).
The present invention compared with the prior art, it is inexpensive that its advantage is that hydrogen sulfide is easy to get, and especially utilizes waste gas hydrogen sulfide in the factory, can turn waste into wealth, and turns harm into good, technology is brief, the product viscosity height, output is also high, cost is low, remarkable in economical benefits is beneficial to industrial production.
Embodiment: in the reactor that need not seal, add sodium hydroxide (content 96%) 12.58 gram and hydrogen sulfide (content 97%) 0.15 molar reactives, add 100 milliliters of hempas again, anhydrous sodium phosphate 24.6 gram, santochlor (content 99%) 22.3 grams, 180-235 ℃ of normal pressure polycondensation 3-4 hour, obtain white or near-white mixture.With the deionized water and the washing with alcohol reaction product of heat, 110-120 ℃ of drying, obtain HMWPPS15.5 gram, yield 95.6%, melt viscosity reaches 6.8 * 10
4Pool (303 ℃ of mensuration).
Claims (3)
1, is the method for raw material synthetic macromolecule amount linear polyphenylthioether with hydrogen sulfide, santochlor and sodium hydroxide, it is characterized in that making auxiliary agent that hempa is made solvent, carry out the polymerization under atmospheric pressure reaction at 180-235 ℃ with anhydrous sodium phosphate.
2,, it is characterized in that the mol amount ratio of santochlor, hydrogen sulfide, sodium hydroxide and anhydrous sodium phosphate is 1～1.02: 1: 2: 0.5-2.20 according to the said method of claim 1.
3,, it is characterized in that said hydrogen sulfide can be that the waste gas hydrogen sulfide and the sulfurous iron ore of discharging in the factory is the hydrogen sulfide of raw material according to claim 1,2 said methods.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85109096A CN85109096B (en) | 1985-12-14 | 1985-12-14 | Synthelization of linear macromolecular polybenzewne thioether |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85109096A CN85109096B (en) | 1985-12-14 | 1985-12-14 | Synthelization of linear macromolecular polybenzewne thioether |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85109096A CN85109096A (en) | 1987-06-24 |
| CN85109096B true CN85109096B (en) | 1988-09-21 |
Family
ID=4796236
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN85109096A Expired CN85109096B (en) | 1985-12-14 | 1985-12-14 | Synthelization of linear macromolecular polybenzewne thioether |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN85109096B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1095481C (en) * | 2000-12-27 | 2002-12-04 | 古旗高 | Process for preparing high-density high-molecular linear polyphenyl thioether |
| CN103897187B (en) | 2012-12-26 | 2015-06-17 | 浙江新和成特种材料有限公司 | Synthesis method of fiber-grade polyphenylene sulfide (PPS) resin |
-
1985
- 1985-12-14 CN CN85109096A patent/CN85109096B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN85109096A (en) | 1987-06-24 |
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