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1, 5-pentyl diisocyanate preparation method

A technology of pentamethylene diisocyanate and butyl pentamethylene dicarbamate, which is applied in the field of preparation of 1,5-pentane diisocyanate to achieve the effects of reduced loss, high purity and high yield

Inactive Publication Date: 2018-10-23
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Purpose of the invention: In order to solve the problem that the raw material 1,5-pentanediamine needs to be refined in the existing 1,5-pentanediisocyanate preparation process, the present invention provides a preparation method of 1,5-pentanediisocyanate

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0022] (1) Lysine fermentation: firstly, transfer the lysine producing strain KA30 glycerol tube to the centrifuge tube for activation culture, then dilute the bacterial solution in the centrifuge tube and smear the plate (peptone 10g / L, yeast powder 5g / L L, sodium chloride 5g / L, agar powder 25g / L, sodium pyruvate 0.5g / L), select single bacterium colony, single bacterium colony is carried out shake flask fermentation verification. After verification, the lysine production strain was inserted into the shake flask for fermentation for 12h (sucrose 20g / L, magnesium sulfate 0.6g / L, potassium dihydrogen phosphate 0.6g / L, ammonium chloride 8.5g / L, yeast powder 6g / L , threonine 0.55g / L, methionine 0.1g / L, monosodium glutamate 7g / L, sodium pyruvate 0.55g / L), sodium hydroxide to adjust the pH to 7.0. Then insert the primary seed medium (consistent with the shake flask medium), control dissolved oxygen 30%-50%, cultivate for about 10h, stop cultivating when the total sugar content drops...

Embodiment 2

[0029] The preparation method is the same as in Example 1, except that the 1,5-pentanediamine n-butanol mixture (the molar ratio of 1,5-pentanediamine and n-butanol is 1:6) does not add n-butanol, urea and The molar ratio of 1,5-pentanediamine is 3:1, the molar ratio of catalyst to 1,5-pentanediamine is 0.5:100, the reaction temperature of carbamateization is 220°C, and the reaction time is 3h, to obtain Butyl pentamethylene dicarbamate (PDU) was 25.37g, the purity was 91.9%, the molar yield was 82.17%, and the molar recovery of n-butanol after vacuum distillation was 69%. The heat carrier selects naphthenic oil, weighs an appropriate amount of naphthenic oil and zinc acetate to make W (heat carrier): W (PDU)=20:1, W (catalyst): W (PDU)=1:100 (mass ratio), The thermal cracking reaction temperature is 270° C., the vacuum degree is set at 0.094 MPa, and the reaction time is 1 h. Finally, 7.98 g of the target product pentamethylene diisocyanate (PDI) was obtained, and the total ...

Embodiment 3

[0031] The preparation method is the same as in Example 1, except that an appropriate amount of n-butanol is added to make the molar ratio of 1,5-pentanediamine and n-butanol reach 1:7, and the molar ratio of urea and 1,5-pentanediamine is 5:1, the consumption and reaction conditions of other substances in the carbamate reaction system are the same as in Example 1, and 25.27g of pentamethylene dicarbamate (PDU) is obtained, the purity is 92.2%, and the molar yield is 82.11 %, n-butanol recovery rate is 73.1%. Heat carrier selects dibutyl phthalate, catalyzer selects zinc powder and zinc oxide, takes by weighing an amount of dioctyl phthalate and zinc powder, zinc oxide, makes W (heat carrier): W (PDU)=15: 1, W (catalyst): W (PDU)=5:100 (wherein the quality of zinc powder and zinc oxide respectively accounts for 50%), thermal cracking reaction reaction condition is the same as embodiment 1, and thermal cracking reaction finishes and finally obtains the target product Wuya Meth...

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Abstract

The invention discloses a 1, 5-pentyl diisocyanate preparation method which includes the steps: (1) mixing 1, 5-pentane diamine transfer solution and extracting solvents, extracting 1, 5-pentane diamine and dewatering extracting solution to obtain mixed solution of the 1, 5-pentane diamine transfer solution and the extracting solvents; (2) adding catalysts and urea into the mixed solution of the 1, 5-pentane diamine transfer solution and the extracting solvents, supplementing an appropriate quantity of extracting solvents to form a reaction system, performing carbamic acid esterification on the 1, 5-pentane diamine and recycling excessive extracting solvents in the reaction system by reduced pressure distillation to obtain PDU; (3) mixing the PDU, heat carriers and the catalysts and performing thermal cracking reaction and separation to obtain the extracting solvents and PDI. According to the method, a large quantity of salts in the transfer solution can be removed by extracting solvent extraction, the extracting solvents can serve as raw materials for synthesizing the PDU, the PDI can be prepared by thermal cracking, and the extracting solvents serving as by-products can be recycled.

Description

technical field [0001] The invention relates to the preparation of 1,5-pentane diisocyanate, in particular to a preparation method of 1,5-pentane diisocyanate. Background technique [0002] Due to its special chemical structure, aliphatic isocyanate (ADI) endows corresponding polyurethane materials with excellent performance. With the rapid development of building materials, painting, automobile and other industries, its application is becoming more and more extensive, and its demand is also increasing year by year. At present, the process route for synthesizing ADI mainly includes phosgene method and non-phosgene method. The phosgene method is a commonly used production method in industry, but the phosgene used in the process of preparing isocyanate by this method is a highly toxic raw material, and a large amount of hydrogen chloride will be released during the reaction, which will easily cause equipment corrosion and environmental pollution. In the non-phosgene process, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C265/14C07C263/04C07C271/20C07C269/04C12P13/00
CPCC12P13/00C07C263/04C07C269/04C07C271/20C07C265/14
Inventor 陈可泉程琪许晟田威龙何育美
Owner NANJING UNIV OF TECH
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