Composite plasticizer taking chlorinated glycerol ester as main body as well as preparation method and application thereof

A technology of chloroglycerol ester and compound plasticizer, applied in the field of polymer materials, can solve the problem that the high value-added processing of crude glycerin cannot be completely solved, the diglyceride cannot be used as a plasticizer, and the refining of crude glycerol cannot be eliminated. Steps and other problems, to solve the high-value utilization of direct high conversion rate, increase the chlor-alkali industry chain, and avoid the effect of being unable to handle

Inactive Publication Date: 2018-03-09
SHANDONG YANHAI CONSTR RESOURCES
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Problems solved by technology

[0004] However, using refined glycerin to synthesize triacetin, the raw materials are limited, and refined glycerin must be used, which cannot get rid of the crude glycerin refining step, so that the utilization rate of glycerin components in crude glycerin is low; at the same time, the reaction yield is limited, and the product contains Monoglycerides and diglycerides further reduce the utilization rate of glycerin, while increasing the discharge of by-products and three wastes
Secondly, although there are patents that use crude glycerin to synthesize tricarboxylic acid glycerides (triacetin is one of them) or a mixture of monoglycerides, diglycerides and triglycerides, only tricarboxylic acid glycerides can It can be used as a plasticizer, but the other two types cannot be used. It is also unavoidable to avoid the problems of low utilization rate of glycerin, many by-products, and many three wastes.
Finally, although there are patents mentioning that triglycerides (vegetable oil is also a kind of triglycerides) can increase compatibility through chlorination, it still cannot solve the problem that monoglycerides and diglycerides cannot be used as plasticizers, and then The problem of low glycerol utilization in crude glycerin remains unsolved
Therefore, using the above reported solutions cannot completely solve the problem of direct and efficient high value-added processing of crude glycerol without producing a large number of by-products
Crude glycerin processing still wastes a lot of glycerin
At the same time, glyceryl triacetate, as a mature plasticizer product, is rarely used in the processing of PVC soft products. Used as a plasticizer for PVC soft products

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  • Composite plasticizer taking chlorinated glycerol ester as main body as well as preparation method and application thereof
  • Composite plasticizer taking chlorinated glycerol ester as main body as well as preparation method and application thereof
  • Composite plasticizer taking chlorinated glycerol ester as main body as well as preparation method and application thereof

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preparation example Construction

[0030] In one embodiment of the present invention, the preparation method of the composite plasticizer taking chloroglycerol ester as main body, comprises the following steps:

[0031] A) Put crude glycerin, alkyl acid or benzoic acid, water-carrying agent and esterification catalyst in a reactor, and react at 80-140°C for 2-5 hours to obtain a dark red liquid;

[0032] B) Distilling the dark red liquid under reduced pressure, collecting fractions below 1kPa and above 100°C to obtain an intermediate product;

[0033] C) after mixing the intermediate product with the chlorination catalyst, carry out chlorination reaction with chlorine gas under light to obtain the composite plasticizer initial product;

[0034] D) Adding 3% by weight stabilizer, 0.5% by weight of surfactant and 5%-10% by weight of viscosity reducer to the initial composite plasticizer product to obtain a composite plasticizer product.

[0035] In one embodiment of the present invention, the crude glycerol is a...

Embodiment 1

[0050] Get the crude glycerin 115g of biodiesel by-product (proportioning is: glycerol 81%, water 10%, inorganic salt 3%, other impurity and colored matter 3%), glacial acetic acid 240g, lanthanum chloride 2.2g and acetic acid Put 72g of ethyl ester in a three-necked flask, raise the temperature to 105°C while stirring constantly, and some components will start to evaporate, and the generated water will be separated continuously through the water separator until 3-4 hours later, no more water will be generated, stop reaction;

[0051] Use a mechanical pump for vacuum distillation, collect fractions below 1kPa and above 100°C, and the fractions are colorless liquids with a faint ester aroma;

[0052] Add a mixture of benzoyl peroxide and tert-butyl peroxybenzoate with a mass fraction of 1‰ to this fraction, and under the irradiation of ultraviolet light, when the water bath is maintained at 60-70°C, chlorine gas is introduced to carry out the chlorination reaction, and the reac...

Embodiment 2

[0056] Get crude glycerol 115g (proportioning by weight percentage is: glycerol 82%, water 6%, inorganic salt 4%, other impurity and colored matter 4%), formic acid 184g, tin chloride 4.6g, dichloroethane 80g, constantly While stirring, the temperature is raised to 85°C, and the components begin to evaporate, and the generated water is continuously separated through the water separator until 2-3 hours later, no more water is generated, and the reaction is stopped.

[0057] Use a mechanical pump to carry out vacuum distillation, collect the fraction below 1kPa and above 100°C, the fraction is a colorless liquid with a faint ester aroma.

[0058] Add a mixture of azobisisobutyronitrile and tert-butyl peroxybenzoate with a mass fraction of 1‰ to the fraction, and under the irradiation of an ultraviolet lamp, when the water bath is maintained at 60-70°C, chlorine gas is introduced to carry out the chlorination reaction, After reacting for 1.5 hours, stop feeding the chlorine gas a...

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Abstract

The invention relates to a composite plasticizer taking chlorinated glycerol ester as a main body. The composite plasticizer comprises: a combination of any three or more of formula (1) to formula (6), wherein R1, R2 and R3 represent H, and C1-C5 alkyl or phenyl respectively; 3 weight percent of a stabilizer, 0.5 weight percent of a surfactant and 5-10 weight percent of a viscosity reducer. The invention also provides a preparation method of the composite plasticizer, and the preparation method comprises reacting a biodiesel byproduct namely crude glycerol, alkyl acid or benzoic acid, a water-carrying agent, and an esterification catalyst, and other steps. The plasticizing efficiency of the composite plasticizer provided by the invention can be equivalent to that of dioctyl phthalate (DOP); moreover, the biodiesel byproduct namely crude glycerol is fully utilized, and direct high-value utilization with a high transformation rate of the crude glycerol and the problem that a large numberof byproducts cannot be treated are fundamentally solved at the same time; on the other hand, chlorine can also be utilized to increase the chlorine-alkali industry chain and increase economic benefits; the preparation process of the composite plasticizer is simple and reliable, and a produced plasticizer product is stable in chemical property and good in product processing property, avoids potential dangers at the same time, and is safe and environment-friendly.

Description

technical field [0001] The invention belongs to the field of macromolecular materials, and in particular relates to a novel composite plasticizer, in particular to a composite plasticizer mainly composed of chloroglycerol ester and its preparation method and application. Background technique [0002] In my country, polyvinyl chloride (PVC) is an important raw material for plastic production. In 2009, the national production capacity reached 17.805 million tons, and the actual output was 9.1549 million tons. Various plastic soft products can be made by using PVC resin with different proportions of plasticizers. At present, the domestic production of plasticizers exceeds 1.5 million tons. Among the total consumption of plasticizers, about 90% are used in PVC resins. Among them, the production and consumption of phthalate plasticizers are the largest. . Domestic phthalate plasticizers mainly include dioctyl phthalate (DOP), dibutyl phthalate (DBP), diisononyl phthalate (DINP)...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L85/02C08L71/02C08K5/103C08K5/1515C08K5/42C08K5/12
CPCC08K5/103C08K2201/014C08L85/02C08L71/02C08K5/1515C08K5/42C08K5/12
Inventor 谭德敏孟庆森孙博
Owner SHANDONG YANHAI CONSTR RESOURCES
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