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Improved method for preparing polyaspartic acid esters from 1, 5-pentamethylene diamine salts

A technology of pentamethylenediamine hydrochloride and pentamethylenediamine, which is applied in the directions of polyurea/polyurethane coatings, cyanide reaction preparation, chemical instruments and methods, etc., can solve problems such as affecting the quality of downstream products of resin and reducing resin yield.

Pending Publication Date: 2022-05-13
摩珈(上海)生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And when there is this cyclic impurity in the Asparagine resin of formula (I), the productive rate of resin can be caused to reduce, and can have a strong impact on the quality of this resin and downstream product

Method used

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  • Improved method for preparing polyaspartic acid esters from 1, 5-pentamethylene diamine salts
  • Improved method for preparing polyaspartic acid esters from 1, 5-pentamethylene diamine salts
  • Improved method for preparing polyaspartic acid esters from 1, 5-pentamethylene diamine salts

Examples

Experimental program
Comparison scheme
Effect test

Embodiment A

[0085] Example A: General Materials and Methods

[0086] The following references are used in the examples: Recombinant DNA manipulations generally follow the methods described in: Sambrook et al., 2001 . Restriction enzymes, T4 DNA ligase, Quick DNA Ligation Kit, SanPrep Column DNA Gel Extraction Kit, Plasmid Mini-Prep Kit and agarose were purchased from Sangon Biotech (Shanghai, China). TE buffer contains 10mM Tris-HCl (pH 8.0) and 1mM Na 2 EDTA (pH 8.0). TAE buffer contains 40mM Tris-acetate (pH 8.0) and 2mM Na 2 EDTA.

[0087] In Example B, restriction enzyme digestion was performed in buffer provided by Sangon Biotech.

[0088] A typical restriction enzyme digest contains: 0.8 μg DNA in 8 μL TE, 2 μL restriction enzyme buffer (10x concentration), 1 μL bovine serum albumin (0.1 mg / mL), 1 μL restriction enzyme, and 8 μL LTE. Reactions were incubated for 1 hour at 37°C and analyzed by agarose gel electrophoresis. DNA for cloning experiments was digested, the reaction...

Embodiment B

[0091] Example B: Cloning, expression and activity testing of lysine decarboxylase expressed in Escherichia coli

[0092] The E. coli lysine decarboxylase kdc (2-keto-acid decarboxylase) gene was synthesized and cloned into pET21a (Millipore Sigma, formerly Novagen). The wild-type kdc nucleic acid sequence from Escherichia coli strain BW25113 (E.C.4.1.1.18) is represented by SEQ ID NO: 1, and the amino acid sequence is represented by SEQ ID NO: 2, annotated as lysine decarboxylase.

[0093] The plasmid containing the kdc gene was transformed into BL21(DE3) E. coli cells. Empty plasmid pET21a was also transformed as a negative control. For enzyme expression and characterization experiments, flasks containing 40 mL TB were inoculated at 5% from overnight cultures and shaken. The flask was incubated at 30°C with shaking at 250rpm for 2 hours, then induced to produce protein with 0.2mM isopropyl β-D-1-thiogalactopyranoside (IPTG), and shaken at 30°C Simultaneously an addition...

Embodiment C

[0096] Example C: Fermentation of transformed Escherichia coli overexpressing KDC

[0097] For the present examples, growth medium was prepared as follows: All solutions were prepared in distilled deionized water. LB medium (1L) contains: Bacto TM tryptone (i.e., an enzymatic digest of casein) (10 g), Bacto TM Yeast extract (ie, the water-soluble fraction of autolyzed yeast extract) (5 g), and NaCl (10 g). LB-glucose medium in 1L LB medium contains: Glucose (10g), MgSO 4 (0.12g), and thiamine hydrochloride (0.001g). LB-freezing buffer contains in 1L LB medium: K 2 HPO 4 (6.3g), KH 2 PO 4 (1.8g), MgSO 4 (1.0g), (NH 4 ) 2 SO 4 (0.9g), sodium citrate dihydrate (0.5g), and glycerol (44mL). M9 Salt (1L) Contains: Na 2 HPO 4 (6g), KH 2 PO 4 (3g), NH 4 Cl (1 g), and NaCl (0.5 g). M9 Minimal Medium in 1L M9 Salts contains: D-glucose (10g), MgSO 4 (0.12g), and thiamine hydrochloride (0.001g). Antibiotics were added when appropriate to the following final concentra...

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Abstract

The invention provides a method for preparing free PDA by desalting and purifying PDA hydrochloride obtained by biological fermentation. The method comprises the following steps: converting lysine hydrochloride into PDA hydrochloride by using lysine decarboxylase; preparing the obtained PDA hydrochloride into an aqueous solution, and adding alkali metal hydroxide into the aqueous solution; evaporating under reduced pressure to remove most water; adding a certain amount of lower aliphatic alcohol; filtering out generated chloride; evaporating under reduced pressure to remove most solvent; optionally, repeating the steps of adding the alcohol, filtering out the chloride and evaporating the solvent under reduced pressure for at least one time; and obtaining a free PDA containing a small amount of the alcohol and a very small amount of water. The invention further provides a method for preparing the radix asparagi resin shown in the formula (I) from the PDA hydrochloride obtained through biological fermentation. The method comprises the following steps: enabling diethyl fumarate to react with the obtained free PDA under certain conditions; and carrying out post-treatment on the obtained reaction liquid to obtain the product radix asparagi resin as shown in the formula (I).

Description

technical field [0001] This application relates to the production of a polyaspartate (PAE). More particularly, the present application describes an improved process for the production of polyaspartate from 1,5-pentanediamine hydrochloride using a solvent-free process that can be produced at lower cost, simpler equipment, and High yield to produce polyaspartate (PAE) from free 1,5-pentanediamine, and the content of piperidine impurities is extremely low. Background technique [0002] Polyaspartic Ester (Polyaspartic Ester, PAE), also known as polyaspartic acid resin or aspartic acid resin, is a special type of sterically hindered secondary amine, which can be obtained by polymerizing aspartic acid ester . PAE resin contains two groups of amino group and carboxyl group. It has strong chelating and adsorption functions. It is widely used in bioengineering, pharmaceutical chemical industry, agriculture and forestry planting and other fields. Aspartic acid polymerization produ...

Claims

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Application Information

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IPC IPC(8): C07C227/08C07C229/24C07C209/86C07C211/09C12P13/00C09D175/02
CPCC07C227/08C07C209/86C12P13/001C09D175/02C07C229/24C07C211/09
Inventor 陆成樑刘文杰曹利峰李东泽徐荣归邱贵森
Owner 摩珈(上海)生物科技有限公司
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