CN110922634A - High-viscosity environment-friendly plasticizer and preparation method and application thereof - Google Patents

High-viscosity environment-friendly plasticizer and preparation method and application thereof Download PDF

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Publication number
CN110922634A
CN110922634A CN201911071922.0A CN201911071922A CN110922634A CN 110922634 A CN110922634 A CN 110922634A CN 201911071922 A CN201911071922 A CN 201911071922A CN 110922634 A CN110922634 A CN 110922634A
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viscosity
environment
friendly
parts
chlorine
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步帅
步贺
李小刚
张旺
曹景魏
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Shijiazhuang Dongxiang Chemical Co Ltd
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Shijiazhuang Dongxiang Chemical Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/02Halogenated hydrocarbons
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C17/00Preparation of halogenated hydrocarbons
    • C07C17/093Preparation of halogenated hydrocarbons by replacement by halogens
    • C07C17/10Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/30Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
    • C07C67/307Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by introduction of halogen; by substitution of halogen atoms by other halogen atoms
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/48Polyethers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/10Esters; Ether-esters
    • C08K5/101Esters; Ether-esters of monocarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/04Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08L27/06Homopolymers or copolymers of vinyl chloride
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2101/00Manufacture of cellular products
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant

Abstract

The invention discloses a high-viscosity environment-friendly plasticizer and a preparation method and application thereof, wherein the plasticizer adopts n-alkane and methyl palmitoleate as chlorinated raw materials, and the weight ratio of the raw materials is 3: 7, mixing and preparing; the preparation method comprises the steps of adding n-alkane and methyl palmitate formate into a reaction kettle and carrying out chlorination reaction in a stepwise manner; the high-viscosity environment-friendly plasticizer can be applied to preparation of environment-friendly foam caulking agents. The plasticizer prepared by the invention does not contain short-chain chlorinated paraffin, has light yellow color and no peculiar smell, can inhibit oil precipitation and has excellent low-temperature resistance; the prepared foam has the advantages of environmental protection, high viscosity, good foam pores, no shrinkage, strong controllability, good emulsification effect and stable performance at low temperature.

Description

High-viscosity environment-friendly plasticizer and preparation method and application thereof
Technical Field
The invention relates to the technical field of production and processing of building materials, and particularly relates to a high-viscosity environment-friendly plasticizer as well as a preparation method and application thereof.
Background
The polyurethane foam gap filler has excellent performances of water resistance, thermal expansion and cold contraction resistance, heat insulation, sound insulation and the like, and is widely used for filling and sealing side seams of building doors and windows, expansion joints of members and holes. At present, the main component of a plasticizer of the polyurethane foam gap filler on the market is chlorinated paraffin, the chlorinated paraffin is not easy to biodegrade, the chlorinated paraffin belongs to a non-renewable petrochemical product, and toxic chloride gas can be generated by decomposition after combustion. Chlorinated paraffin containing SCCP short chain has strong toxicity to aquatic organisms, brings long-term negative effects to aquatic environment, has carcinogenic possibility to human beings, and affects immune system and reproductive system of human body.
2017, 10 and 27, and a carcinogen list published by the international cancer research institution of the world health organization is preliminarily collated and referred to as follows: chlorinated paraffins with an average carbon chain length of 12 and an average degree of chlorination of about 60% are on the class 2B carcinogen list.
The conventional 52# chlorinated paraffin has high chlorination degree, but has small viscosity (the viscosity is 160-300mpa.s) after chlorination, reduces the speed of full drying, and the prepared foam is easy to collapse; the palmitoleic acid methyl ester has low chlorination degree, large viscosity and strong rigidity after chlorination, and causes foam shrinkage, poor fluidity and easy solidification; the existing first-line high-viscosity chlorinated paraffin on the market is medium-long carbon chain chlorinated paraffin, has high viscosity and high density, so that the compatibility is poor, therefore, manufacturers can only achieve proper viscosity and density by adding short-chain alkane, the performances of high viscosity and good qualification are achieved in performance, the cost is reduced, but the adding of short-chain alkane generates SCCP, influences the ecological environment and is unfavorable for the health development of human beings. Therefore, an environment-friendly plasticizer with relatively high viscosity is needed to adjust the setting effect of the foam.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: the high-viscosity environment-friendly plasticizer is provided to solve the problem that proper viscosity and density can be obtained only by adding short-chain chlorinated paraffin which affects the ecological environment and is unfavorable for the human health development as the plasticizer in the foam joint mixture, so that the ecological environment is improved and the production cost is reduced on the basis of not reducing the viscosity of the foam joint mixture.
In order to solve the technical problems, the invention provides a high-viscosity environment-friendly plasticizer.
A high-viscosity environment-friendly plasticizer adopts C14-C16Straight-chain n-alkanes and methyl palmitoleate are chlorinated starting materials in the weight ratio of 3: 7 in a certain proportion.
The chlorine content of the high-viscosity environment-friendly plasticizer is 45-55%, and the density is 1.20-1.28g/cm at 50 DEG C3The viscosity is 650-850 mpa.s.
The invention also provides a preparation method of the high-viscosity environment-friendly plasticizer, which comprises the following steps:
a1: n-alkanes and methyl palm olein formate were mixed as 3: 7, mixing uniformly, and putting into a reaction kettle;
a2: under the catalysis of illumination, 30m of gas is introduced3The flow rate of the vaporized chlorine is per hour, and the temperature is raised to 75 ℃ after the chlorine is introduced for 4 hours;
a3: increase chlorine flow to 40m3Introducing chlorine for 6 hours, and controlling the temperature at 75-85 ℃;
a4: chlorine flow rate maintenance of 40m3H, controlling the temperature to be 75-85 ℃, and reacting for 12 hours;
a5: chlorine flow rate maintenance of 40m3H, raising the temperature to 85-95 ℃, and reacting for 18 hours;
a6: chlorine flow rate maintenance of 40m3H, raising the temperature to 95-105 ℃, and reacting for 40 hours;
a7: detecting whether the density and the viscosity of the plasticizer reach the standard or not, blowing off hydrogen chloride after the density and the viscosity reach the standard, detecting that the acid value is less than or equal to 0.15mgKOH/g, and adding 0.3 percent of diglycidyl ether serving as a composite heat stabilizer to obtain the high-viscosity environment-friendly plasticizer.
Further, the normal alkane in A1 is C14-C16Straight-chain normal alkanes.
Further, the illumination in A2 adopts a black light lamp with the wavelength of 330-400 nm.
The invention also provides an application method of the high-viscosity environment-friendly plasticizer, which is used for preparing the environment-friendly foam joint mixture, wherein the environment-friendly foam joint mixture comprises the following components in parts by weight:
5-10 parts of polyether polyol, 25-75 parts of high-viscosity environment-friendly plasticizer, 0.5-3 parts of silicone oil foam stabilizer, 0.3-0.8 part of dimorpholinyl diethyl ether, 15-30 parts of isocyanate, 5-10 parts of dimethyl ether and 5-10 parts of propane and butane.
Due to the adoption of the technical scheme, the technical progress of the invention is as follows.
C of the invention which will have very good compatibility14-C16The high-viscosity environment-friendly plasticizer is prepared by mixing and reacting straight-chain n-alkane and methyl palmitoleate according to a proportion, wherein C is chloridized14-C16The straight-chain normal alkane has the advantages of high chlorination degree, controllable degree and capability of achieving ideal density; the high-viscosity environment-friendly plasticizer is light yellow in color, has no peculiar smell, can inhibit oil precipitation, has excellent low-temperature resistance, and can be normally used in winter. The high-viscosity environment-friendly plasticizer disclosed by the invention does not contain short-chain chlorinated paraffin, can be used for preparing an environment-friendly polyurethane foam gap filler, adopts novel degradable methyl palmitoleate to replace a large amount of direct-connected alkane, replaces a petroleum product with natural renewable energy, is more environment-friendly, and has the characteristics of good cells, no shrinkage, strong controllability, good emulsification effect and stable performance at low temperature.
In addition, the high-viscosity environment-friendly plasticizer is also suitable for the PVC industry, and the produced plastic product has high mechanical property, excellent gelling capacity, saponification resistance, low migration resistance, good resistance performance, obvious stability at low temperature and high flame retardance.
Detailed Description
The invention provides a high-viscosity environment-friendly plasticizer and a preparation method and application thereof, wherein the high-viscosity environment-friendly plasticizer adopts C14-C16Straight-chain n-alkanes and methyl palmitoleate are chlorinated starting materials in the weight ratio of 3: 7 in a certain proportion.
The chlorine content of the high-viscosity environment-friendly plasticizer is 45-55%, and the density is 1.20-1.28g/cm at 50 DEG C3The viscosity is 650-850 mpa.s.
The preparation method of the high-viscosity environment-friendly plasticizer comprises the following specific steps:
a1: will be C14-C16Linear n-alkanes and palm oil methyl formate according to 3: 7, mixing uniformly, and putting into a reaction kettle;
a2: catalyzing under the illumination of a black light lamp with the wavelength of 330-400nm, and introducing 30m3The flow rate of the vaporized chlorine is per hour, and the temperature is raised to 75 ℃ after the chlorine is introduced for 4 hours;
a3: increase chlorine flow to 40m3Introducing chlorine for 6 hours, and controlling the temperature at 75-85 ℃;
a4: chlorine flow rate maintenance of 40m3H, controlling the temperature to be 75-85 ℃, and reacting for 12 hours;
a5: chlorine flow rate maintenance of 40m3H, raising the temperature to 85-95 ℃, and reacting for 18 hours;
a6: chlorine flow rate maintenance of 40m3H, raising the temperature to 95-105 ℃, and reacting for 40 hours;
a7: detecting whether the density of the chlorinated paraffin reaches 1.20-1.28g/cm3And whether the viscosity reaches 650-850mpa.s, blowing dehydrochlorination for 8-10 hours after the viscosity reaches the standard, detecting that the acid value is less than or equal to 0.15mgKOH/g, and adding 0.3 percent of diglycidyl ether serving as a composite heat stabilizer to obtain the high-viscosity environment-friendly plasticizer.
The high-viscosity environment-friendly plasticizer can be applied to preparation of an environment-friendly foam gap filler, and the environment-friendly foam gap filler is composed of the following components in parts by weight:
5-10 parts of polyether polyol, 25-75 parts of high-viscosity environment-friendly plasticizer, 0.5-3 parts of silicone oil foam stabilizer, 0.3-0.8 part of dimorpholinyl diethyl ether, 15-30 parts of isocyanate, 5-10 parts of dimethyl ether and 5-10 parts of propane and butane.
The present invention will be described in further detail with reference to specific examples.
Example 1
The high viscosity environment friendly plasticizer has chlorine content of 45-55% and density of 1.20-1.28g/cm at 50 deg.c3The viscosity is 650-850 mpa.s.
The high-viscosity environment-friendly plasticizer comprises the following specific preparation steps:
a1: will be C14-C16Linear n-alkanes and palm oil methyl formate according to 3: 7, mixing uniformly, and putting into a reaction kettle;
a2: catalyzing under the illumination of a black light lamp with the wavelength of 330-400nm, and introducing 30m3The flow rate of the vaporized chlorine is per hour, and the temperature is raised to 75 ℃ after the chlorine is introduced for 4 hours;
a3: increase chlorine flow to 40m3Introducing chlorine for 6 hours, and controlling the temperature at 80 ℃;
a4: chlorine flow rate maintenance of 40m3H, controlling the temperature at 85 ℃ and reacting for 12 hours;
a5: chlorine flow rate maintenance of 40m3H, raising the temperature to 95 ℃ and reacting for 18 hours;
a6: chlorine flow rate maintenance of 40m3H, raising the temperature to 105 ℃, and reacting for 40 hours;
a7: the density of the chlorinated paraffin is detected to be 1.25g/cm3And the viscosity is 750mpa.s, the hydrogen chloride is blown off for 8 hours, the acid value is detected to be less than or equal to 0.15mgKOH/g, and 0.3 percent of diglycidyl ether of composite heat stabilizer is added to obtain the high-viscosity environment-friendly plasticizer.
The high-viscosity environment-friendly plasticizer can be applied to preparation of an environment-friendly foam joint mixture, and the environment-friendly foam joint mixture is composed of the following components in parts by weight: 6 parts of polyether polyol, 25 parts of high-viscosity environment-friendly plasticizer, 3 parts of silicone oil foam stabilizer, 0.7 part of dimorpholinyl diethyl ether, 30 parts of isocyanate, 7 parts of dimethyl ether and 6.5 parts of propane and butane.
Example 2
The high viscosity environment friendly plasticizer has chlorine content of 45-55% and density of 1.20-1.28g/cm at 50 deg.c3The viscosity is 650-850 mpa.s.
The high-viscosity environment-friendly plasticizer comprises the following specific preparation steps:
a1: will be C14-C16Linear n-alkanes and palm oil methyl formate according to 3: 7, mixing uniformly, and putting into a reaction kettle;
a2: catalyzing under the illumination of a black light lamp with the wavelength of 330-400nm, and introducing 30m3The flow rate of the vaporized chlorine is per hour, and the temperature is raised to 75 ℃ after the chlorine is introduced for 4 hours;
a3: increase chlorine flow to 40m3Introducing chlorine for 6 hours, and controlling the temperature at 75 ℃;
a4: chlorine flow rate maintenance of 40m3H, controlling the temperature at 79 ℃ and reacting for 12 hours;
a5: chlorine flow rate maintenance of 40m3H, raising the temperature to 85 ℃ and reacting for 18 hours;
a6: chlorine flow rate maintenance of 40m3H, raising the temperature to 100 ℃ and reacting for 40 hours;
a7: the density of the chlorinated paraffin is detected to be 1.25g/cm3And the viscosity is 810mpa.s, the hydrogen chloride is blown off for 10 hours, the acid value is detected to be less than or equal to 0.15mgKOH/g, and 0.3 percent of diglycidyl ether of composite heat stabilizer is added to obtain the high-viscosity environment-friendly plasticizer.
The high-viscosity environment-friendly plasticizer can be applied to preparation of an environment-friendly foam joint mixture, and the environment-friendly foam joint mixture is composed of the following components in parts by weight: 5 parts of polyether polyol, 75 parts of high-viscosity environment-friendly plasticizer, 1 part of silicone oil foam stabilizer, 0.4 part of dimorpholinyl diethyl ether, 25 parts of isocyanate, 10 parts of dimethyl ether and 9.4 parts of propane and butane.
Example 3
The high viscosity environment friendly plasticizer has chlorine content of 45-55% and density of 1.20-1.28g/cm at 50 deg.c3The viscosity is 650-850 mpa.s.
The high-viscosity environment-friendly plasticizer comprises the following specific preparation steps:
a1: will be C14-C16Linear n-alkanes and palm oil methyl formate according to 3: 7, mixing uniformly, and putting into a reaction kettle;
a2: catalyzing under the illumination of a black light lamp with the wavelength of 330-400nm, and introducing 30m3The flow rate of the vaporized chlorine is per hour, and the temperature is raised to 75 ℃ after the chlorine is introduced for 4 hours;
a3: increase chlorine flow to 40m3Introducing chlorine for 6 hours, and controlling the temperature at 75 ℃;
a4: chlorine flow rate maintenance of 40m3H, controlling the temperature at 83 ℃ and reacting for 12 hours;
a5: chlorine flow rate maintenance of 40m3H, raising the temperature to 95 ℃ and reacting for 18 hours;
a6: chlorine flow rate maintenance of 40m3H, raising the temperature to 105 ℃, and reacting for 40 hours;
a7: the density of the chlorinated paraffin is detected to be 1.23g/cm3And the viscosity is 670mpa.s, the hydrogen chloride is blown off for 8 hours, the acid value is detected to be less than or equal to 0.15mgKOH/g, and 0.3 percent of diglycidyl ether of composite heat stabilizer is added to obtain the high-viscosity environment-friendly plasticizer.
The high-viscosity environment-friendly plasticizer can be applied to preparation of an environment-friendly foam joint mixture, and the environment-friendly foam joint mixture is composed of the following components in parts by weight: 8 parts of polyether polyol, 60 parts of high-viscosity environment-friendly plasticizer, 0.5 part of silicone oil foam stabilizer, 0.3 part of dimorpholinyl diethyl ether, 15 parts of isocyanate, 8 parts of dimethyl ether and 5 parts of propane and butane.
Example 4
The high viscosity environment friendly plasticizer has chlorine content of 45-55% and density of 1.20-1.28g/cm at 50 deg.c3The viscosity is 650-850 mpa.s.
The high-viscosity environment-friendly plasticizer comprises the following specific preparation steps:
a1: will be C14-C16Linear n-alkanes and palm oil methyl formate according to 3: 7, mixing uniformly, and putting into a reaction kettle;
a2: catalyzing under the illumination of a black light lamp with the wavelength of 330-400nm, and introducing 30m3The flow rate of the vaporized chlorine is per hour, and the temperature is raised to 75 ℃ after the chlorine is introduced for 4 hours;
a3: increase chlorine flow to 40m3Introducing chlorine for 6 hours, and controlling the temperature at 77 ℃;
a4: chlorine flow rate maintenance of 40m3H, controlling the temperature at 83 ℃ and reacting for 12 hours;
a5: chlorine flow rate maintenance of 40m3H, raising the temperature to 90 ℃ and reacting for 18 hours;
a6: chlorine flow rate maintenance of 40m3H, raising the temperature to 105 ℃, and reacting for 40 hours;
a7: the density of the chlorinated paraffin is detected to be 1.26g/cm3And the viscosity is 730mpa.s, the hydrogen chloride is blown off for 8 hours, the acid value is detected to be less than or equal to 0.15mgKOH/g, and 0.3 percent of diglycidyl ether of composite heat stabilizer is added to obtain the high-viscosity environment-friendly plasticizer.
The high-viscosity environment-friendly plasticizer can be applied to preparation of an environment-friendly foam joint mixture, and the environment-friendly foam joint mixture is composed of the following components in parts by weight: 9 parts of polyether polyol, 50 parts of high-viscosity environment-friendly plasticizer, 2 parts of silicone oil foam stabilizer, 0.8 part of dimorpholinyl diethyl ether, 23 parts of isocyanate, 5 parts of dimethyl ether and 10 parts of propane and butane.
Example 5
The high viscosity environment friendly plasticizer has chlorine content of 45-55% and density of 1.20-1.28g/cm at 50 deg.c3The viscosity is 650-850 mpa.s.
The high-viscosity environment-friendly plasticizer comprises the following specific preparation steps:
a1: will be C14-C16Linear n-alkanes and palm oil methyl formate according to 3: 7, mixing uniformly, and putting into a reaction kettle;
a2: catalyzing under the illumination of a black light lamp with the wavelength of 330-400nm, and introducing 30m3The flow rate of the vaporized chlorine is per hour, and the temperature is raised to 75 ℃ after the chlorine is introduced for 4 hours;
a3: increase chlorine flow to 40m3/h,Introducing chlorine for 6 hours, and controlling the temperature at 75 ℃;
a4: chlorine flow rate maintenance of 40m3H, controlling the temperature at 80 ℃ and reacting for 12 hours;
a5: chlorine flow rate maintenance of 40m3H, raising the temperature to 95 ℃ and reacting for 18 hours;
a6: chlorine flow rate maintenance of 40m3H, raising the temperature to 100 ℃ and reacting for 40 hours;
a7: the density of the chlorinated paraffin is detected to be 1.28g/cm3And the viscosity is 650mpa.s, the hydrogen chloride is blown off for 10 hours, the acid value is detected to be less than or equal to 0.15mgKOH/g, and 0.3 percent of diglycidyl ether of composite heat stabilizer is added to obtain the high-viscosity environment-friendly plasticizer.
The high-viscosity environment-friendly plasticizer can be applied to preparation of an environment-friendly foam joint mixture, and the environment-friendly foam joint mixture is composed of the following components in parts by weight: 10 parts of polyether polyol, 35 parts of high-viscosity environment-friendly plasticizer, 1.7 parts of silicone oil foam stabilizer, 0.5 part of dimorpholinyl diethyl ether, 17 parts of isocyanate, 6 parts of dimethyl ether and 7.0 parts of propane and butane.
The high-viscosity environment-friendly plasticizers prepared in examples 1 to 5 were subjected to SCCP test and viscosity test, respectively.
1) And (3) SCCP detection:
the high-viscosity environment-friendly plasticizer prepared by the invention and the glue prepared by the high-viscosity environment-friendly plasticizer prepared by the invention are respectively referred to ISO 18219:2015, and gas chromatography-tandem mass spectrometry is adopted for detection, and the detection result shows that the plasticizer prepared by the invention has no SCCP and does not harm the ecological environment.
2) And (3) viscosity detection:
the viscosity of the high-viscosity environment-friendly plasticizer prepared in five examples was measured and compared with the viscosity of the conventional plasticizer. The results are shown in the table I:
viscosity (Unit: mpa.s)
1 2 3 4 5 Mean value of
Comparative example 710 720 750 730 710 724
Examples 780 770 770 780 770 774
The experimental data show that the viscosity average value of the high-viscosity environment-friendly plasticizer prepared by the invention reaches 774mpa.s, and compared with the viscosity average value 724mpa.s of the existing plasticizer, the viscosity average value is greatly improved, the deviation is small, and the product performance is stable.

Claims (5)

1. High-viscosity environment-friendlyA plasticizer characterized by: by C14-C16Straight-chain n-alkanes and methyl palmitoleate are chlorinated starting materials in the weight ratio of 3: 7, mixing and preparing;
the chlorine content of the high-viscosity environment-friendly plasticizer is 45-55%, and the density is 1.20-1.28g/cm at 50 DEG C3The viscosity is 650-850 mpa.s.
2. The preparation method of the high-viscosity environment-friendly plasticizer according to claim 1, which comprises the following steps:
a1: n-alkanes and methyl palm olein formate were mixed as 3: 7, mixing uniformly, and putting into a reaction kettle;
a2: under the catalysis of illumination, 30m of gas is introduced3The flow rate of the vaporized chlorine is per hour, and the temperature is raised to 75 ℃ after the chlorine is introduced for 4 hours;
a3: increase chlorine flow to 40m3Introducing chlorine for 6 hours, and controlling the temperature at 75-85 ℃;
a4: chlorine flow rate maintenance of 40m3H, controlling the temperature to be 75-85 ℃, and reacting for 12 hours;
a5: chlorine flow rate maintenance of 40m3H, raising the temperature to 85-95 ℃, and reacting for 18 hours;
a6: keeping the chlorine flow at 40m3/h, raising the temperature to 95-105 ℃, and reacting for 40 hours;
a7: detecting whether the density and the viscosity of the plasticizer reach the standard or not, blowing off hydrogen chloride after the density and the viscosity reach the standard, detecting that the acid value is less than or equal to 0.15mgKOH/g, and adding 0.3 percent of diglycidyl ether serving as a composite heat stabilizer to obtain the high-viscosity environment-friendly plasticizer.
3. The method for preparing high-viscosity environment-friendly plasticizer according to claim 2, wherein said n-alkane in A1 is C14-C16Straight-chain normal alkanes.
4. The method for preparing high viscosity environment-friendly plasticizer according to claim 2, wherein the illumination in A2 is performed by a black light lamp with a wavelength of 330-400 nm.
5. The use of the high-viscosity environment-friendly plasticizer according to any one of claims 1 to 4, for preparing an environment-friendly foam gap filler, wherein the environment-friendly foam gap filler comprises the following components in parts by weight:
5-10 parts of polyether polyol, 25-75 parts of high-viscosity environment-friendly plasticizer, 0.5-3 parts of silicone oil foam stabilizer, 0.3-0.8 part of dimorpholinyl diethyl ether, 15-30 parts of isocyanate, 5-10 parts of dimethyl ether and 5-10 parts of propane and butane.
CN201911071922.0A 2019-11-05 2019-11-05 High-viscosity environment-friendly plasticizer and preparation method and application thereof Pending CN110922634A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021212703A1 (en) * 2020-04-20 2021-10-28 山东岩海建设资源有限公司 Chlorinated fatty acid ester environment-friendly plasticizer and preparation method therefor
CN116082947A (en) * 2022-12-06 2023-05-09 石家庄东翔化工有限公司 Low-viscosity polyurethane quick-drying spray coating and preparation method and application thereof

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