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Method of preparing cellulose acetate butyrate by means of dichloromethane solvent method

A technology of dichloromethane and acetic acid butyric acid, which is applied in the field of preparation of cellulose acetate butyrate, can solve problems such as paint film embrittlement and cold cracking, and achieve the effects of reducing waste water volume, reducing consumption, and stabilizing product quality indicators

Inactive Publication Date: 2017-07-25
JIANGSU RUICHEN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For those thermoplastic film-forming substances where cellulose acetate butyrate is not crosslinked, the use of very low molecular weight cellulose acetate butyrate as a modifier and additive may cause embrittlement of the paint film, cold cracking and related defects

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: The purpose of this embodiment is to utilize dichloromethane solvent to prepare cellulose acetate butyrate. The specific operation steps are as follows: (1) spray acetic acid on the wood pulp and activate it at normal temperature for 6-12h; , butyric anhydride, butyric acid, sulfuric acid catalyst, after mixing evenly, cool down to 5-20 ℃ for use; the consumption of the mixture is 2-3 times of the consumption of wood pulp; the consumption of sulfuric acid catalyst is 1% of the consumption of wood pulp -2%.

[0029] (2) all the materials in (1) are dropped into the esterification still that has dichloromethane solvent, carry out esterification, control reaction time between 30-90min; Add magnesium acetate solution, stir evenly, then add acetic acid diluted solution whose consumption is 1-2 times of the consumption of wood pulp to it, and the diluted solution is discharged into the hydrolysis kettle; the consumption of described methylene chloride is the con...

Embodiment 2

[0033]Embodiment 2: the difference between this embodiment and embodiment 1 is that in this embodiment, the addition amount of the acetic acid solution in step (3) is 1-3 times of the wood pulp consumption. The consumption of methylene chloride in step (2) is 3-5 times of the consumption of wood pulp, and the temperature of esterification reaction is between 40-55 DEG C; During step (3) hydrolysis, control the water content in the system at 8-15 %between.

Embodiment 3

[0034] Embodiment 3: a kind of preparation method of high viscosity cellulose acetate butyrate comprises the steps:

[0035] Step 1: Spray 100 parts of acetic acid evenly into 100 parts of wood pulp, activate at room temperature for 6-12 hours; cool the mixture of acetic anhydride, butyric anhydride, butyric acid and sulfuric acid catalyst to 5°C-10°C Use; The mixture is 200-300 parts;

[0036] Step 2: Put all the materials in step 1 and the solvent dichloromethane into the esterification tank to carry out the esterification reaction. The esterification reaction temperature is 46°C-50°C, and the reaction time is controlled within 40-80min; Add neutralizing liquid magnesium acetate to neutralize 50% of the catalyst, then add 100-150 parts of acetic acid with a mass fraction of 67% for dilution, and discharge the diluted slurry into the hydrolysis tank;

[0037] Step 3: Add 100-300 parts of acetic acid with a mass fraction of 67% to the hydrolysis kettle for hydrolysis, control...

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Abstract

The invention discloses a method of preparing cellulose acetate butyrate by means of a dichloromethane solvent method. The method comprises the following steps: (1) spraying acetic acid to wood pulp and performing activation at constant temperature; in addition, uniformly mixing acetic anhydride, butyric anhydride, butyric acid and a sulfuric acid catalyst; (2) inputting the material in an esterification kettle with a dichloromethane solvent for esterification reaction, after reaction, adding magnesium acetate into the reaction system, uniformly stirring the mixture, adding acetic acid into the mixture to dilute, and discharging the diluted solution into a hydrolysis kettle; (3) adding acetic acid into the hydrolysis kettle to promote hydrolysis, wherein the temperature of the system is 60-85 DEG C, and the time is controlled within 3-7h; and after hydrolysis, adding magnesium acetate into the system; and (4) performing filter pressing, performing flash evaporation on the filtrate, adding water for chromatography, and performing washing and drying. By this way, the cellulose acetate butyrate, the dynamic viscosity of which is 5000cps-7000cps, is obtained. The method is simple in operating step, high in controllability, good in atom economy, safe in operating environment and small in wastewater quantity.

Description

technical field [0001] The invention relates to the field of chemical preparation, in particular to a preparation method of cellulose acetate butyrate. Background technique [0002] Cellulose acetate is used as an additive in many coatings to give them many good properties, but it lacks the solubility range, miscibility and moisture resistance necessary for some coatings. After cellulose acetate butyrate is introduced into butyl ester, it has a wider solubility range and miscibility than pure cellulose acetate. It is not only soluble in common solvents such as acetone, but also soluble in organic acids, methyl isobutyl ketone, butyl acetate Solvent systems such as esters and ethyl acetate, cellulose acetate butyrate with a high degree of substitution of butyl esters can even be dissolved in ethanol and other alcohol solvents, which makes it widely used in the coating industry to improve the fluidity and leveling of coatings Performance, outdoor durability, pigment control, ...

Claims

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Application Information

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IPC IPC(8): C08B3/18
CPCC08B3/18
Inventor 陈祥宋宇飞钱建强陈伟张勇钱冬
Owner JIANGSU RUICHEN CHEM
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