Polymerization method of (ammonium) sulfate connexon polymer

A linker and polymer technology, applied in the field of polymer materials

Pending Publication Date: 2019-12-06
内蒙古图微新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Another object of the present invention is to provide a kind of high-performance bisphenol type polysulfate (urethane) ester polymer material for the problems (for example, problems such as stability) existing in the polyester material

Method used

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  • Polymerization method of (ammonium) sulfate connexon polymer
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  • Polymerization method of (ammonium) sulfate connexon polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0094] Example 1. Synthesis of polysulfate-1 containing 4,4-dihydroxydiphenyl with a degree of polymerization of 5-1000.

[0095] (1) Synthesis of sulfonyl fluoride-protected bisphenol: Dissolve 228 g (1 mol) of bisphenol A in 100 mL of dichloromethane or chloroform solution, add 24.2 g (2.40 mol) of triethylamine, and then carefully and continuously add Sulfonyl fluoride gas. The reaction was carried out at room temperature for 12 hours. After the reaction was completed, 388 g of sulfonyl fluoride-protected bisphenol A (the full English name of 1,4-phenylene bis(sulfurofluoridate)) was obtained as a dark brown solid after simple concentration, filtration and washing. The yield was : 99%.

[0096] NMR data of the synthesized product: 1 H NMR (400MHz, CDCl 3 )δ7.36–7.15(m, 8H), 1.69(s, 6H).13C NMR (400MHz, CDCl) 3 )δ150.44, 148.20, 128.74, 120.61, 42.95, 30.75

[0097] The structural formula of the synthesized product is as follows:

[0098]

[0099] Experiments show t...

Embodiment 2

[0113] Example 2. Synthesis of polysulfate PSE-2 (PSE-2) containing 4,4-dihydroxydiphenyl ether with a degree of polymerization of 5 to 500

[0114] (1) Synthesis of bisphenol A protected by sulfonyl fluoride: same as Example 1.

[0115] (2) Synthesis of Bisphenol Polysulfate-2 (PSE-2) with a Degree of Polymerization of 10 to 500

[0116]

[0117] Under nitrogen protection, 392 g (10 mol) of sulfonyl fluoride-protected bisphenol A prepared above and 202 g (10 mol) of 4,4-dihydroxydiphenyl ether in an equal molar amount, 300 g of NMP solvent, and 50 g of xylene were heated. After completely dissolving, add 120% molar weight (1.2mol) of catalyst potassium carbonate, react under mechanical stirring at 130 ° C for 2 hours, heat up to 170 ° C and react for 12 hours, then pour the mixture into water to terminate the reaction, and separate the precipitated polymer product. , extracted with ethanol and dried to obtain 4,4-dihydroxydiphenyl-containing polysulfate PSE-2 as a white sol...

Embodiment 3

[0119] Example 3. Synthesis of polysulfate PSE-3 (PSE-3) containing 4,4-dihydroxydiphenyl sulfide with a degree of polymerization of 5 to 500

[0120] (1) Synthesis of bisphenol A protected by sulfonyl fluoride: same as Example 1.

[0121] (2) Synthesis of Bisphenol Polysulfate-3 (PSE-3) with a Degree of Polymerization of 10 to 500

[0122]

[0123] Under nitrogen protection, 392 g (10 mol) of sulfonyl fluoride-protected bisphenol A prepared above and 218 g (10 mol) of 4,4-dihydroxydiphenyl sulfide in an equal molar amount, 300 g of NMP solvent, and 50 g of xylene were prepared. After heating to dissolve completely, add 120% molar weight (1.2mol) of catalyst potassium carbonate, react at 130 ° C under mechanical stirring for 2 hours, heat up to 170 ° C and react for 12 hours, then pour the mixture into water to terminate the reaction, and separate the precipitated polymerization. The product was extracted with ethanol and dried to obtain 4,4-dihydroxydiphenyl-containing po...

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Abstract

The invention relates to a polymerization method of an (ammonium) sulfate connexon polymer. The polymerization method comprises a step of subjecting a hydroxyl-containing monomer or an amino-containing monomer and a sulfuryl fluoride monomer to condensation polymerization on through a one-pot process under alkaline conditions. Compared with a traditional polyester synthesis method, the method is cost-saving; reaction conditions are mild and easy to control; reaction flow is simple, and operation is easy; and a post-treatment process is simple, environmental pollution is small, and industrial production is facilitated. In addition, a bisphenol type polysulfate compound synthesized in the invention has excellent mechanical properties, dielectric properties, tolerance and wear resistance.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, in particular, a sulfuric acid (amine) ester polymer is constructed through a polycondensation reaction of phenol, alcohol or amino group with sulfonyl fluoride or sulfuryl fluoride under the action of alkali. Background technique [0002] With the continuous progress of science and technology, as one of the important chemical synthetic materials, the polyester industry has achieved rapid development in recent years. At present, polyester materials have been widely used in fiber manufacturing, packaging, engineering plastics, electronic appliances, medical materials, construction, automobiles and other fields. In comparison, polyester materials have the advantages of relatively simple and controllable synthesis, high utilization rate of raw material monomers, and lower cost. Therefore, polyester materials have been widely used in industrial production and people's daily life. [0003]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/26
CPCC08G75/26C08G75/24C08G65/4006C08G75/23C08G65/40C08G75/30
Inventor 蒋先兴周云斌
Owner 内蒙古图微新材料科技有限公司
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