Method for synthesizing homopolymer N-vinyl butyrolactam with super-low molecular weight and super-low residual monomer

Patent metadata

Field	Value
Publication number	US-9453087-B2
Application number	US-201214401743-A
Country	US
Kind code	B2
Filing date	Jul 23, 2012
Priority date	May 16, 2012
Publication date	Sep 27, 2016
Grant date	Sep 27, 2016

Abstract

A synthesis method of ultra low molecular weight homopolymerized N-vinyl butyrolactam with ultra low residual monomer content is provided N-vinyl butyrolactam monomers and water are provided with the mass ratio of 3:17˜8:12 0.5%˜5.0% by weight of initiators, 0.1%˜5.0% by weight of a catalyst, and 0.1%˜10% by weight of a molecular weight regulator are provided in the presence of an inert gas, adding the above mentioned raw materials in batches, adjusting the pH of the reaction system to 7.0-8.0 with an activator, reacting at the polymerization temperature of 60-85° C. A peroxide is added and maintaining the temperature for 2 hours, to obtain an aqueous solution of ultra low molecular weight homopolymerized N-vinyl butyrolactam. The aqueous solution is dried to obtain a powdery ultra low molecular weight homopolymerized N-vinyl butyrolactam with ultra low residual monomer content.

First claim

We claim:

1. A synthesis method of ultra low molecular weight homopolymerized N-vinyl butyrolactam with ultra low residual monomer content comprising:
providing N-vinyl butyrolactam monomers and water with the mass ratio of 3:17˜8:12, then based on the N-vinyl butyrolactam monomers, providing 0.5%˜5.0% by weight of initiators, 0.1%˜5.0% by weight of a catalyst, and 0.1%˜10% by weight of a molecular weight regulator, wherein the initiators include 25% by weight of the weight of initiators of an initiator A, 67.5% by weight of the weight of initiators of an initiator B and 7.5% by weight of the weight of initiators of an initiator C;
in the presence of an inert gas, first adding 45% of the total weight of the water, 30% of the total weight of the N-vinyl butyrolactam monomers, the initiator A, 70% of the total weight of the catalyst and at least 70% of the total weight of the molecular weight regulator, adjusting the pH of the reaction system to 7.0-8.0 with an activator, reacting at the polymerization temperature of 60-85° C., adding the remaining water, the remaining N-vinyl butyrolactam monomers, the initiator B, the remaining catalyst and the remaining molecular weight regulator in batches during the initial 4-9 hours after the beginning of the reaction, adjusting the pH of the reaction system to 7.0-8.0 with the activator during this period, then adding the initiator C after keeping the temperature of 80-100° C. for 30 minutes, then adding a peroxide with 0.01% ˜1% of the total weight of the N-vinyl butyrolactam monomers after keeping the temperature for 1-3 hours, then further keeping the temperature for 2 hours, to obtain an aqueous solution of ultra low molecular weight homopolymerized N-vinyl butyrolactam, drying the aqueous solution to obtain a powdery ultra low molecular weight homopolymerized N-vinyl butyrolactam with ultra low residual monomer content, whose K value is 12-17, whose weight average molecular weight is 2000-15000, and whose residual monomer content is less than 10 ppm.

2. The synthesis method of ultra low molecular weight homopolymerized N-vinyl butyrolactam with ultra low residual monomer content according to claim 1 , wherein the initiators are selected from the group consisting of: hydrogen peroxide, tert-butyl hydroperoxide, tert-amyl hydroperoxide, peroxydisulfuric, and potassium peroxydisulfate.

3. The synthesis method of ultra low molecular weight homopolymerized N-vinyl butyrolactam with ultra low residual monomer content according to claim 2 , wherein the initiator A is a solution mixing hydrogen peroxide and tert-butyl hydroperoxide; the initiator B is tert-butyl hydroperoxide or a solution mixing hydrogen peroxide and tert-butyl hydroperoxide; the initiator C is tert-butyl hydroperoxide or a solution mixing hydrogen peroxide and tert-butyl hydroperoxide.

4. The synthesis method of ultra low molecular weight homopolymerized N-vinyl butyrolactam with ultra low residual monomer content according to claim 1 , wherein the catalyst is selected from at least one of ferrous sulfate aqueous solution, ferrous chloride aqueous solution and copper sulfate aqueous solution.

5. The synthesis method of ultra low molecular weight homopolymerized N-vinyl butyrolactam with ultra low residual monomer content according to claim 1 , wherein the molecular weight regulator is selected from at last one of ethanol, n-propanol, isopropanol, dodecyl mercaptan and sulfite.

6. The synthesis method of ultra low molecular weight homopolymerized N-vinyl butyrolactam with ultra low residual monomer content according to claim 1 , wherein the activator is ammonia water, sodium hydroxide, triethanolamine, hydroxyl ammonium salt or sodium carbonate.

7. The synthesis method of ultra low molecular weight homopolymerized N-vinyl butyrolactam with ultra low residual monomer content according to claim 1 , wherein the peroxide is hydrogen peroxide or tert-butyl hydroperoxide.

Assignees

• Wang Yu
• Liu Wei
• Chen Zhan
• Shanghai Yuking Water Soluble Mat Tech Co Ltd

Inventors

• Wang Yu
• Liu Wei
• Chen Zhan

Classifications

• C08F126/06 Primary

  by a heterocyclic ring containing nitrogen · CPC title

• C08F4/38

  Mixtures of peroxy-compounds · CPC title

• C08F6/003

  from polymer solutions, suspensions, dispersions or emulsions without recovery of the polymer therefrom · CPC title

• C08F24/00 Primary

  Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a heterocyclic ring containing oxygen (cyclic esters of polyfunctional acids C08F18/00; cyclic anhydrides of unsaturated acids C08F20/00, C08F22/00) · CPC title

• C08L39/04

  Homopolymers or copolymers of monomers containing heterocyclic rings having nitrogen as ring member · CPC title