# US 10,308,764 B2 · Method for preparing biobased nylon: polylactam

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- Number: US 10,308,764 B2
- Document ID: US10308764B2
- Status: Granted
- Kind: B2
- Application number: 15/542,602
- Filed: 2015-07-13
- Published: 2018-08-09
- Granted: 2019-06-04
- Earliest claimed: 2015-01-08
- Assignees: East China University of Science and Technology
- Applicants: East China University of Science and Technology
- Inventors: Liming Zhao; Jie Wei; Jun Qian; Juan Ma; Xiaofeng Tang; Yingyang Wu; Yongjun Qiu
- Web page: https://patentgrep.com/patent/US10308764B2

## CPC

- C08G 69/16: Preparatory processes
- C08G 69/24: Pyrrolidones or piperidones
- C12P 13/005: {Amino acids other than alpha- or beta amino acids, e.g. gamma amino acids}
- C12Y 401/01015: Glutamate decarboxylase (4.1.1.15)
- C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C12P: FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE {(brewing of beer C12C; producing vinegar C12J; producing specific peptides or proteins C07K; producing enzymes C12N9/00; DNA or RNA concerning genetic engineering, vectors, e.g. plasmids, or their isolation, preparation or purification C12N15/00; measuring or testing processes involving enzymes or microorganisms C12Q; measuring or testing processes involving nucleic acid amplification reactions C12Q1/6844; fermentation processes to form a food composition, A21 or A23; compounds in general, see the relevant compound class, e.g. C01, C07)}
- C12Y: ENZYMES

## Abstract

The invention relates to a preparation method of green nylon poly butyrolactams, the biological materials of GABA in vacuum under the condition of high temperature melt decomposition and purified butyrolactams, then by vacuum polymerization of green nylon poly butyrolactams. Compared with the prior art, the invention is prepared by biological method for the synthesis of a wide range of sources, to solve the problem of raw material supply PA4 for mass production, reduce the cost of reaction, and the reaction condition is simple, easy to implement simplified synthesis steps, from the laboratory to the transformation of industrial production.

## Claims

### Claim 1

A method for preparing a green nylon polybutyrolactam, comprising:
obtaining a purified butyrolactam from processes including melting γ-aminobutyric acid and vacuum purification of butyrolactam; and
obtaining a green nylon polybutyrolactam from a process including vacuum polymerization of the purified butyrolactam.

### Claim 2 (depends on 1)

The method according to claim 1,
wherein the process of melting γ-aminobutyric acid includes stirring the γ-aminobutyric acid under nitrogen atmosphere and melting γ-aminobutyric acid at a temperature of 200-225° C. to obtain an oily liquid containing a small amount of water;
the process of vacuum purification includes vacuum drying the oily liquid in a vacuum chamber at a temperature of 70° C.;
the process of vacuum polymerization includes:
adding a catalyst to the purified butyrolactam in a reactor and flowing nitrogen to remove air in the reactor,
heating the purified butyrolactam in an oil bath to a temperature of 50° C., and stirring until the catalyst reacts with the purified butyrolactam,
adding an initiator and reacting for 8-15 hours to obtain a reaction product,
washing the reaction product with water and acetone, and
drying the reaction product to obtain green nylon polybutyrolactam.

### Claim 3 (depends on 2)

The method according to claim 2, wherein γ-aminobutyric acid is obtained from a process including fermenting a biomass, conducting enzymatic conversion with glutamic acid decarboxylase, and performing extraction and purification.

### Claim 4 (depends on 2)

The method according to claim 2, wherein the method is conducted under a nitrogen atmosphere with a nitrogen flow rate of 3-5 ml/min.

### Claim 5 (depends on 2)

The method according to claim 2, wherein a mass ratio of the butyrolactam, the catalyst, and the initiator in the process of vacuum polymerization is 1:(0.25-0.375):(0.5-0.75).

### Claim 6 (depends on 2)

The method according to claim 2, wherein the catalyst includes sodium, sodium hydroxide, or potassium hydroxide.

### Claim 7 (depends on 2)

The method according to claim 2, wherein the initiator includes benzoyl chloride or sebacoyl chloride.

### Claim 8 (depends on 1)

The method according to claim 1, further comprising adding formic acid to cap a termini of the green nylon polybutyrolactam.

### Claim 9 (depends on 2)

The method according to claim 2, wherein the purified butyrolactam has a purity of higher than 99.6%.

### Claim 10 (depends on 2)

The method according to claim 2, wherein the green nylon polybutyrolactam has a molecular weight of 10,000.