CN109082250A - A kind of preparation method of harsh thermosol formula - Google Patents

A kind of preparation method of harsh thermosol formula Download PDF

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Publication number
CN109082250A
CN109082250A CN201810754507.4A CN201810754507A CN109082250A CN 109082250 A CN109082250 A CN 109082250A CN 201810754507 A CN201810754507 A CN 201810754507A CN 109082250 A CN109082250 A CN 109082250A
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parts
weight
tpr
solution viscosity
reaches
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林进森
林上炜
卢军朝
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Kunshan Taitian New Materials Co Ltd
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Kunshan Taitian New Materials Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J153/00—Adhesives based on block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
    • C09J153/02—Vinyl aromatic monomers and conjugated dienes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08—Macromolecular additives
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
    • C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
    • C09J123/04—Homopolymers or copolymers of ethene
    • C09J123/08—Copolymers of ethene
    • C09J123/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
    • C09J123/0853—Vinylacetate
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J157/00—Adhesives based on unspecified polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C09J157/02—Copolymers of mineral oil hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The present invention relates to a kind of preparation method of harsh thermosol formula, the by weight EVA of 10-30%, the resin of 10-50%, the wax of the TPR of 15-60%, 5-30%, the antiagers of 1-5%；The resin is C9 hydrogenated petroleum resin and terpene resin, the wax is PX-105, the antiager is by four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester and phosphorous acid three (2,4- di-tert-butyl-phenyl) ester composition, be sufficiently stirred makes uniformly to mix in a kettle, then grinds pelletizing, production requirement is harsh, guarantees the excellent performance of micelle finished product.

Description

A kind of preparation method of harsh thermosol formula
Technical field
The present invention relates to a kind of preparation method of EVA hot-melt adhesive formula, especially a kind of system of harsh thermosol formula Preparation Method.
Background technique
Ethylene-vinyl acetate copolymer (Ethylene-Vinyl Acetate, EVA) product of rubber and plastic is novel environment friendly plastics Material, have many advantages, such as good antidetonation, it is moisture-proof, buffering, it is heat-insulated, have it is nontoxic, do not absorb water.Be widely used in wire and cable, The fields such as functional greenhouse film, foaming shoe material, packaging film, hot melt adhesive and toy.
But it since ethylene-vinyl acetate copolymer main component is EVA, due to requiring more excellent performance, produces It is required that more harsh, for this purpose, we have developed a kind of formula of hot melt adhesive, micelle is had excellent performance, and production requirement is harsh.
Summary of the invention
A kind of preparation side of harsh thermosol formula is provided the invention aims to overcome the deficiencies in the prior art Method, it is desirable that it is harsh, guarantee micelle end properties.
In order to achieve the above objectives, the technical solution adopted by the present invention is that: a kind of preparation method of harsh thermosol formula, Characterized by the following steps:
Step 1: prepare each raw material component by weight:
The ethylene/vinyl acetate copolymer resins and EVA of 10-30%, the ethylene/vinyl acetate copolymer resins account for 53.3%, the EVA account for the C9 hydrogenated petroleum resin and terpene resin of 46.7%, 10-50%, the Fischer-Tropsch wax PX- of 5-30% 105,15-60% TPR (Thermo-Plastic-Rubber material) thermoplastic rubber material, the TPR are benzene second The solution viscosity of alkene-isoprene-styrene block copolymer, the TPR half is 1430, and the solution viscosity of half is 1600,1-5% antiager；The antiager is by four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters It is formed with (2, the 4- di-tert-butyl-phenyl) ester of phosphorous acid three；
The portion for being 43.9% by the ethylene/vinyl acetate copolymer resins parts by weights, 56.1% portion；It will be described EVA parts by weights is two parts of 50%；By three parts that the Fischer-Tropsch wax parts by weights is 26.3%, 21.1% portion；It is described The weight that C9 hydrogenated petroleum resin accounts for resin is 93.7%, is divided into four parts of 19.84%, 20.6% portion；The terpenes tree The weight that rouge accounts for resin is 6.3%, a；The TPR parts by weights that the solution viscosity is 1600 is two parts of 39%, 21.9% Portion；The TPR parts by weights that the solution viscosity is 1430 is two parts of 39%, 21.9% portion；The antiager is pressed Parts by weight are divided into 0.1% described four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters and 0.1% institute State phosphorous acid three (2,4- di-tert-butyl-phenyl) ester.
Step 2: sequentially feed intake refining
(1) oil temperature is set as 195 DEG C, material temperature is set as 135 DEG C；It adjusts oil temperature and reaches 160 DEG C, material temperature reaches 130 DEG C When be added that the TPR that the solution viscosity of 39% parts by weight is 1600 is a, the solution viscosity of 39% parts by weight is 1430 TPR it is a, the ethylene/vinyl acetate copolymer resins of 43.9% parts by weight are a, the 19.84% C9 non-hydrogenated petroleum Resin is a, and 2.8% terpene resin is a, and 0.1% described four [β-(3,5- di-t-butyl -4- hydroxy benzenes are added Base) propionic acid] pentaerythritol ester and 0.1% the phosphorous acid three (2,4- di-tert-butyl-phenyl) ester, stirring makes object in reaction kettle Material uniformly mixing, heating melting；
(2) after twenty minutes, it adjusts oil temperature and reaches 195 DEG C, the solution of 39% parts by weight is added in material temperature when reaching 132 DEG C The TPR that viscosity is 1600 is a, and the TPR that the solution viscosity of 39% parts by weight is 1430 is a, 50% parts by weight it is described EVA is a, and the Fischer-Tropsch wax of 26.3% parts by weight is a；
(3) it after above step (2) feeds intake 35 minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 133 DEG C The TPR that the solution viscosity of 21.9% parts by weight is 1600 is a, and the solution viscosity of 21.9% parts by weight is 1430 TPR is a, and the ethylene/vinyl acetate copolymer resins of 56.1% parts by weight are a, the C9 hydrogenation of 19.84% parts by weight Petropols are a；
(4) it after above step (3) feeds intake 50 minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 132 DEG C The C9 hydrogenated petroleum resin of 19.84% parts by weight is a, and the Fischer-Tropsch wax of 26.3% parts by weight is a, 50% parts by weight The EVA it is a；
(5) above step (4) feeds intake after sixty minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 133 DEG C The C9 hydrogenated petroleum resin of 19.84% parts by weight is a, and the Fischer-Tropsch wax of 26.3% parts by weight is a；
(6) it after above step (5) feeds intake 70 minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 132 DEG C The C9 hydrogenated petroleum resin of 20.6% parts by weight is a, and the Fischer-Tropsch wax of 21.1% parts by weight is a.
Step 3: excision forming
For the control of Melt Pump feed side pressure in 3.3-3.8 atmospheric pressure, Melt Pump discharges lateral pressure control at 1.9-2.2 Atmospheric pressure, engine speed 22-26RPM, cutter rotating velocity 1700-1900RPM, output material grain after step 2 terminates 90 minutes.
Due to the application of the above technical scheme, compared with the prior art, the invention has the following advantages:
The preparation method of harsh thermosol formula of the present invention, the by weight EVA of 10-30%, the tree of 10-50% Rouge, the wax of the TPR of 15-60%, 5-30%, the antiager of 1-5%；The resin be C9 hydrogenated petroleum resin and terpene resin, The wax is PX-105, and the antiager is by four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters and Asia Tricresyl phosphate (2,4- di-tert-butyl-phenyl) ester composition, be sufficiently stirred makes uniformly to mix in a kettle, then grinds pelletizing, it is desirable that tight It is severe, guarantee micelle end properties.
Specific embodiment
The present invention will now be described in detail with reference to examples.
Embodiment one
A kind of preparation method of harsh thermosol formula, it is characterised in that the following steps are included:
Step 1: prepare each raw material component by weight:
The ethylene/vinyl acetate copolymer resins and EVA of 10-30%, the ethylene/vinyl acetate copolymer resins account for 53.3%, the EVA account for the C9 hydrogenated petroleum resin and terpene resin of 46.7%, 10-50%, the Fischer-Tropsch wax PX- of 5-30% 105,15-60% TPR (Thermo-Plastic-Rubber material) thermoplastic rubber material, the TPR are benzene second The solution viscosity of alkene-isoprene-styrene block copolymer, the TPR half is 1430, and the solution viscosity of half is 1600,1-5% antiager；The antiager is by four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters It is formed with (2, the 4- di-tert-butyl-phenyl) ester of phosphorous acid three；
The portion for being 43.9% by the ethylene/vinyl acetate copolymer resins parts by weights, 56.1% portion；It will be described EVA parts by weights is two parts of 50%；By three parts that the Fischer-Tropsch wax parts by weights is 26.3%, 21.1% portion；It is described The weight that C9 hydrogenated petroleum resin accounts for resin is 93.7%, is divided into four parts of 19.84%, 20.6% portion；The terpenes tree The weight that rouge accounts for resin is 6.3%, a；The TPR parts by weights that the solution viscosity is 1600 is two parts of 39%, 21.9% Portion；The TPR parts by weights that the solution viscosity is 1430 is two parts of 39%, 21.9% portion；The antiager is pressed Parts by weight are divided into 0.1% described four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters and 0.1% institute State phosphorous acid three (2,4- di-tert-butyl-phenyl) ester.
Step 2: sequentially feed intake refining
(1) oil temperature is set as 195 DEG C, material temperature is set as 135 DEG C；It adjusts oil temperature and reaches 160 DEG C, material temperature reaches 130 DEG C When be added that the TPR that the solution viscosity of 39% parts by weight is 1600 is a, the solution viscosity of 39% parts by weight is 1430 TPR it is a, the ethylene/vinyl acetate copolymer resins of 43.9% parts by weight are a, the 19.84% C9 non-hydrogenated petroleum Resin is a, and 2.8% terpene resin is a, and 0.1% described four [β-(3,5- di-t-butyl -4- hydroxy benzenes are added Base) propionic acid] pentaerythritol ester and 0.1% the phosphorous acid three (2,4- di-tert-butyl-phenyl) ester, stirring makes object in reaction kettle Material uniformly mixing, heating melting；
(2) after twenty minutes, it adjusts oil temperature and reaches 195 DEG C, the solution of 39% parts by weight is added in material temperature when reaching 132 DEG C The TPR that viscosity is 1600 is a, and the TPR that the solution viscosity of 39% parts by weight is 1430 is a, 50% parts by weight it is described EVA is a, and the Fischer-Tropsch wax of 26.3% parts by weight is a；
(3) it after above step (2) feeds intake 35 minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 133 DEG C The TPR that the solution viscosity of 21.9% parts by weight is 1600 is a, and the solution viscosity of 21.9% parts by weight is 1430 TPR is a, and the ethylene/vinyl acetate copolymer resins of 56.1% parts by weight are a, the C9 hydrogenation of 19.84% parts by weight Petropols are a；
(4) it after above step (3) feeds intake 50 minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 132 DEG C The C9 hydrogenated petroleum resin of 19.84% parts by weight is a, and the Fischer-Tropsch wax of 26.3% parts by weight is a, 50% parts by weight The EVA it is a；
(5) above step (4) feeds intake after sixty minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 133 DEG C The C9 hydrogenated petroleum resin of 19.84% parts by weight is a, and the Fischer-Tropsch wax of 26.3% parts by weight is a；
(6) it after above step (5) feeds intake 70 minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 132 DEG C The C9 hydrogenated petroleum resin of 20.6% parts by weight is a, and the Fischer-Tropsch wax of 21.1% parts by weight is a.
Step 3: excision forming
For the control of Melt Pump feed side pressure in 3.3-3.8 atmospheric pressure, Melt Pump discharges lateral pressure control at 1.9-2.2 Atmospheric pressure, engine speed 22-26RPM, cutter rotating velocity 1700-1900RPM, output material grain after step 2 terminates 90 minutes.
Embodiment two
A kind of preparation method of harsh thermosol formula, it is characterised in that the following steps are included:
Step 1: prepare each raw material component by weight:
10% ethylene/vinyl acetate copolymer resins and EVA, the ethylene/vinyl acetate copolymer resins account for 53.3%, institute It states EVA and accounts for 46.7%, 10% C9 hydrogenated petroleum resin and terpene resin, 15% Fischer-Tropsch wax PX-105,60% TPR (Thermo-Plastic-Rubber materia1) thermoplastic rubber material, the TPR are styrene-isoprene-benzene second Alkene block copolymer, the solution viscosity of the TPR half are 1430, and the solution viscosity of half is 1600,5% antiager；Institute Antiager is stated by four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters and (2, the 4- bis- tertiary fourths of phosphorous acid three Base phenyl) ester composition；
The portion for being 43.9% by the ethylene/vinyl acetate copolymer resins parts by weights, 56.1% portion；It will be described EVA parts by weights is two parts of 50%；By three parts that the Fischer-Tropsch wax parts by weights is 26.3%, 21.1% portion；It is described The weight that C9 hydrogenated petroleum resin accounts for resin is 93.7%, is divided into four parts of 19.84%, 20.6% portion；The terpenes tree The weight that rouge accounts for resin is 6.3%, a；The TPR parts by weights that the solution viscosity is 1600 is two parts of 39%, 21.9% Portion；The TPR parts by weights that the solution viscosity is 1430 is two parts of 39%, 21.9% portion；The antiager is pressed Parts by weight are divided into 0.1% described four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters and 0.1% institute State phosphorous acid three (2,4- di-tert-butyl-phenyl) ester.
Step 2: sequentially feed intake refining
(1) oil temperature is set as 195 DEG C, material temperature is set as 135 DEG C；It adjusts oil temperature and reaches 160 DEG C, material temperature reaches 130 DEG C When be added that the TPR that the solution viscosity of 39% parts by weight is 1600 is a, the solution viscosity of 39% parts by weight is 1430 TPR it is a, the ethylene/vinyl acetate copolymer resins of 43.9% parts by weight are a, the 19.84% C9 non-hydrogenated petroleum Resin is a, and 2.8% terpene resin is a, and 0.1% described four [β-(3,5- di-t-butyl -4- hydroxy benzenes are added Base) propionic acid] pentaerythritol ester and 0.1% the phosphorous acid three (2,4- di-tert-butyl-phenyl) ester, stirring makes object in reaction kettle Material uniformly mixing, heating melting；
(2) after twenty minutes, it adjusts oil temperature and reaches 195 DEG C, the solution of 39% parts by weight is added in material temperature when reaching 132 DEG C The TPR that viscosity is 1600 is a, and the TPR that the solution viscosity of 39% parts by weight is 1430 is a, 50% parts by weight it is described EVA is a, and the Fischer-Tropsch wax of 26.3% parts by weight is a；
(3) it after above step (2) feeds intake 35 minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 133 DEG C The TPR that the solution viscosity of 21.9% parts by weight is 1600 is a, and the solution viscosity of 21.9% parts by weight is 1430 TPR is a, and the ethylene/vinyl acetate copolymer resins of 56.1% parts by weight are a, the C9 hydrogenation of 19.84% parts by weight Petropols are a；
(4) it after above step (3) feeds intake 50 minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 132 DEG C The C9 hydrogenated petroleum resin of 19.84% parts by weight is a, and the Fischer-Tropsch wax of 26.3% parts by weight is a, 50% parts by weight The EVA it is a；
(5) above step (4) feeds intake after sixty minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 133 DEG C The C9 hydrogenated petroleum resin of 19.84% parts by weight is a, and the Fischer-Tropsch wax of 26.3% parts by weight is a；
(6) it after above step (5) feeds intake 70 minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 132 DEG C The C9 hydrogenated petroleum resin of 20.6% parts by weight is a, and the Fischer-Tropsch wax of 21.1% parts by weight is a.
Step 3: excision forming
For the control of Melt Pump feed side pressure in 3.3-3.8 atmospheric pressure, Melt Pump discharges lateral pressure control at 1.9-2.2 Atmospheric pressure, engine speed 22-26RPM, cutter rotating velocity 1700-1900RPM, output material grain after step 2 terminates 90 minutes.
Embodiment three
A kind of preparation method of harsh thermosol formula, it is characterised in that the following steps are included:
Step 1: prepare each raw material component by weight:
30% ethylene/vinyl acetate copolymer resins and EVA, the ethylene/vinyl acetate copolymer resins account for 53.3%, institute It states EVA and accounts for 46.7%, 49% C9 hydrogenated petroleum resin and terpene resin, 5% Fischer-Tropsch wax PX-105,15% TPR (Thermo-Plastic-Rubber material) thermoplastic rubber material, the TPR are styrene-isoprene-benzene second Alkene block copolymer, the solution viscosity of the TPR half are 1430, and the solution viscosity of half is 1600,1% antiager；Institute Antiager is stated by four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters and (2, the 4- bis- tertiary fourths of phosphorous acid three Base phenyl) ester composition；
The portion for being 43.9% by the ethylene/vinyl acetate copolymer resins parts by weights, 56.1% portion；It will be described EVA parts by weights is two parts of 50%；By three parts that the Fischer-Tropsch wax parts by weights is 26.3%, 21.1% portion；It is described The weight that C9 hydrogenated petroleum resin accounts for resin is 93.7%, is divided into four parts of 19.84%, 20.6% portion；The terpenes tree The weight that rouge accounts for resin is 6.3%, a；The TPR parts by weights that the solution viscosity is 1600 is two parts of 39%, 21.9% Portion；The TPR parts by weights that the solution viscosity is 1430 is two parts of 39%, 21.9% portion；The antiager is pressed Parts by weight are divided into 0.1% described four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters and 0.1% institute State phosphorous acid three (2,4- di-tert-butyl-phenyl) ester.
Step 2: sequentially feed intake refining
(1) oil temperature is set as 195 DEG C, material temperature is set as 135 DEG C；It adjusts oil temperature and reaches 160 DEG C, material temperature reaches 130 DEG C When be added that the TPR that the solution viscosity of 39% parts by weight is 1600 is a, the solution viscosity of 39% parts by weight is 1430 TPR it is a, the ethylene/vinyl acetate copolymer resins of 43.9% parts by weight are a, the 19.84% C9 non-hydrogenated petroleum Resin is a, and 2.8% terpene resin is a, and 0.1% described four [β-(3,5- di-t-butyl -4- hydroxy benzenes are added Base) propionic acid] pentaerythritol ester and 0.1% the phosphorous acid three (2,4- di-tert-butyl-phenyl) ester, stirring makes object in reaction kettle Material uniformly mixing, heating melting；
(2) after twenty minutes, it adjusts oil temperature and reaches 195 DEG C, the solution of 39% parts by weight is added in material temperature when reaching 132 DEG C The TPR that viscosity is 1600 is a, and the TPR that the solution viscosity of 39% parts by weight is 1430 is a, 50% parts by weight it is described EVA is a, and the Fischer-Tropsch wax of 26.3% parts by weight is a；
(3) it after above step (2) feeds intake 35 minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 133 DEG C The TPR that the solution viscosity of 21.9% parts by weight is 1600 is a, and the solution viscosity of 21.9% parts by weight is 1430 TPR is a, and the ethylene/vinyl acetate copolymer resins of 56.1% parts by weight are a, the C9 hydrogenation of 19.84% parts by weight Petropols are a；
(4) it after above step (3) feeds intake 50 minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 132 DEG C The C9 hydrogenated petroleum resin of 19.84% parts by weight is a, and the Fischer-Tropsch wax of 26.3% parts by weight is a, 50% parts by weight The EVA it is a；
(5) above step (4) feeds intake after sixty minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 133 DEG C The C9 hydrogenated petroleum resin of 19.84% parts by weight is a, and the Fischer-Tropsch wax of 26.3% parts by weight is a；
(6) it after above step (5) feeds intake 70 minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 132 DEG C The C9 hydrogenated petroleum resin of 20.6% parts by weight is a, and the Fischer-Tropsch wax of 21.1% parts by weight is a.
Step 3: excision forming
For the control of Melt Pump feed side pressure in 3.3-3.8 atmospheric pressure, Melt Pump discharges lateral pressure control at 1.9-2.2 Atmospheric pressure, engine speed 22-26RPM, cutter rotating velocity 1700-1900RPM, output material grain after step 2 terminates 90 minutes.
Example IV
A kind of preparation method of harsh thermosol formula, it is characterised in that the following steps are included:
Step 1: prepare each raw material component by weight:
18% ethylene/vinyl acetate copolymer resins and EVA, the ethylene/vinyl acetate copolymer resins account for 53.3%, institute It states EVA and accounts for 46.7%, 44% C9 hydrogenated petroleum resin and terpene resin, 16% Fischer-Tropsch wax PX-105,21% TPR (Thermo-Plastic-Rubber material) thermoplastic rubber material, the TPR are styrene-isoprene-benzene second Alkene block copolymer, the solution viscosity of the TPR half are 1430, and the solution viscosity of half is 1600,1% antiager；Institute Antiager is stated by four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters and (2, the 4- bis- tertiary fourths of phosphorous acid three Base phenyl) ester composition；
The portion for being 43.9% by the ethylene/vinyl acetate copolymer resins parts by weights, 56.1% portion；It will be described EVA parts by weights is two parts of 50%；By three parts that the Fischer-Tropsch wax parts by weights is 26.3%, 21.1% portion；It is described The weight that C9 hydrogenated petroleum resin accounts for resin is 93.7%, is divided into four parts of 19.84%, 20.6% portion；The terpenes tree The weight that rouge accounts for resin is 6.3%, a；The TPR parts by weights that the solution viscosity is 1600 is two parts of 39%, 21.9% Portion；The TPR parts by weights that the solution viscosity is 1430 is two parts of 39%, 21.9% portion；The antiager is pressed Parts by weight are divided into 0.1% described four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters and described 0.1% Phosphorous acid three (2,4- di-tert-butyl-phenyl) ester.
Step 2: sequentially feed intake refining
(1) oil temperature is set as 195 DEG C, material temperature is set as 135 DEG C；It adjusts oil temperature and reaches 160 DEG C, material temperature reaches 130 DEG C When be added that the TPR that the solution viscosity of 39% parts by weight is 1600 is a, the solution viscosity of 39% parts by weight is 1430 TPR it is a, the ethylene/vinyl acetate copolymer resins of 43.9% parts by weight are a, the 19.84% C9 non-hydrogenated petroleum Resin is a, and 2.8% terpene resin is a, and 0.1% described four [β-(3,5- di-t-butyl -4- hydroxy benzenes are added Base) propionic acid] pentaerythritol ester and 0.1% the phosphorous acid three (2,4- di-tert-butyl-phenyl) ester, stirring makes object in reaction kettle Material uniformly mixing, heating melting；
(2) after twenty minutes, it adjusts oil temperature and reaches 195 DEG C, the solution of 39% parts by weight is added in material temperature when reaching 132 DEG C The TPR that viscosity is 1600 is a, and the TPR that the solution viscosity of 39% parts by weight is 1430 is a, 50% parts by weight it is described EVA is a, and the Fischer-Tropsch wax of 26.3% parts by weight is a；
(3) it after above step (2) feeds intake 35 minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 133 DEG C The TPR that the solution viscosity of 21.9% parts by weight is 1600 is a, and the solution viscosity of 21.9% parts by weight is 1430 TPR is a, and the ethylene/vinyl acetate copolymer resins of 56.1% parts by weight are a, the C9 hydrogenation of 19.84% parts by weight Petropols are a；
(4) it after above step (3) feeds intake 50 minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 132 DEG C The C9 hydrogenated petroleum resin of 19.84% parts by weight is a, and the Fischer-Tropsch wax of 26.3% parts by weight is a, 50% parts by weight The EVA it is a；
(5) above step (4) feeds intake after sixty minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 133 DEG C The C9 hydrogenated petroleum resin of 19.84% parts by weight is a, and the Fischer-Tropsch wax of 26.3% parts by weight is a；
(6) it after above step (5) feeds intake 70 minutes, adjusts oil temperature and reaches 195 DEG C, addition when material temperature reaches 132 DEG C The C9 hydrogenated petroleum resin of 20.6% parts by weight is a, and the Fischer-Tropsch wax of 21.1% parts by weight is a.
Step 3: excision forming
For the control of Melt Pump feed side pressure in 3.3-3.8 atmospheric pressure, Melt Pump discharges lateral pressure control at 1.9-2.2 Atmospheric pressure, engine speed 22-26RPM, cutter rotating velocity 1700-1900RPM, output material grain after step 2 terminates 90 minutes.
The above is only specific application examples of the invention, are not limited in any way to protection scope of the present invention.All uses Equivalent transformation or equivalent replacement and the technical solution formed, all fall within rights protection scope of the present invention.

Claims (1)

1. a kind of preparation method of harsh thermosol formula, it is characterised in that the following steps are included:
Step 1: prepare each raw material component by weight:
The ethylene/vinyl acetate copolymer resins and EVA of 10-30%, the ethylene/vinyl acetate copolymer resins account for 53.3%, institute State C9 hydrogenated petroleum resin and terpene resin that EVA accounts for 46.7%, 10-50%, the Fischer-Tropsch wax PX-105,15-60% of 5-30% TPR (Thermo-Plastic-Rubber material) thermoplastic rubber material, the TPR be styrene-isoprene- Styrene block copolymer, the solution viscosity of the TPR half are 1430, and the solution viscosity of half is the anti-ageing of 1600,1-5% Agent；The antiager is by four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters and phosphorous acid three (2,4- bis- Tert-butyl-phenyl) ester composition；
The portion for being 43.9% by the ethylene/vinyl acetate copolymer resins parts by weights, 56.1% portion；By the EVA Parts by weights is two parts of 50%；By three parts that the Fischer-Tropsch wax parts by weights is 26.3%, 21.1% portion；The C9 hydrogen The weight that fossil oleoresin accounts for resin is 93.7%, is divided into four parts of 19.84%, 20.6% portion；The terpene resin accounts for The weight of resin is 6.3%, a；The TPR parts by weights that the solution viscosity is 1600 is two parts of 39%, the one of 21.9% Part；The TPR parts by weights that the solution viscosity is 1430 is two parts of 39%, 21.9% portion；The antiager is by weight Part is divided into 0.1% described four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters and 0.1% Asia Tricresyl phosphate (2,4- di-tert-butyl-phenyl) ester.
Step 2: sequentially feed intake refining
(1) oil temperature is set as 195 DEG C, material temperature is set as 135 DEG C；It adjusts oil temperature and reaches 160 DEG C, material temperature adds when reaching 130 DEG C The TPR that the solution viscosity for entering 39% parts by weight is 1600 is a, the TPR that the solution viscosity of 39% parts by weight is 1430 The ethylene/vinyl acetate copolymer resins of portion, 43.9% parts by weight are a, the 19.84% C9 hydrogenated petroleum resin Portion, 2.8% terpene resin is a, and 0.1% described four [β-(3,5- di-tert-butyl-hydroxy phenyl) third are added Acid] pentaerythritol ester and 0.1% the phosphorous acid three (2,4- di-tert-butyl-phenyl) ester, stirring keeps material uniform in reaction kettle Mixing, heating melting；
(2) after twenty minutes, it adjusts oil temperature and reaches 195 DEG C, the solution viscosity of 39% parts by weight is added in material temperature when reaching 132 DEG C A for 1600 TPR, the TPR that the solution viscosity of 39% parts by weight is 1430 is a, the EVA mono- of 50% parts by weight Part, the Fischer-Tropsch wax of 26.3% parts by weight is a；
(3) it after above step (2) feeds intake 35 minutes, adjusts oil temperature and reaches 195 DEG C, 21.9% weight is added in material temperature when reaching 133 DEG C The TPR that the solution viscosity for measuring part is 1600 is a, and the TPR that the solution viscosity of 21.9% parts by weight is 1430 is a, The ethylene/vinyl acetate copolymer resins of 56.1% parts by weight are a, the C9 hydrogenated petroleum resin of 19.84% parts by weight It is a；
(4) it after above step (3) feeds intake 50 minutes, adjusts oil temperature and reaches 195 DEG C, 19.84% weight is added in material temperature when reaching 132 DEG C The C9 hydrogenated petroleum resin for measuring part is a, and the Fischer-Tropsch wax of 26.3% parts by weight is a, the EVA of 50% parts by weight It is a；
(5) above step (4) feeds intake after sixty minutes, adjusts oil temperature and reaches 195 DEG C, 19.84% weight is added in material temperature when reaching 133 DEG C The C9 hydrogenated petroleum resin for measuring part is a, and the Fischer-Tropsch wax of 26.3% parts by weight is a；
(6) it after above step (5) feeds intake 70 minutes, adjusts oil temperature and reaches 195 DEG C, 20.6% weight is added in material temperature when reaching 132 DEG C The C9 hydrogenated petroleum resin for measuring part is a, and the Fischer-Tropsch wax of 21.1% parts by weight is a.
Step 3: excision forming
For the control of Melt Pump feed side pressure in 3.3-3.8 atmospheric pressure, Melt Pump discharges lateral pressure control in 1.9-2.2 atmosphere Pressure, engine speed 22-26RPM, cutter rotating velocity 1700-1900RPM, output material grain after step 2 terminates 90 minutes.
CN201810754507.4A 2018-07-11 2018-07-11 A kind of preparation method of harsh thermosol formula Pending CN109082250A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996003470A1 (en) * 1994-07-26 1996-02-08 Exxon Chemical Patents Inc. Hot melt adhesive based on eva and styrene block polymers
CN101880517A (en) * 2010-07-19 2010-11-10 杭州天创化学技术有限公司 Low-temperature resistant hot melt glue

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996003470A1 (en) * 1994-07-26 1996-02-08 Exxon Chemical Patents Inc. Hot melt adhesive based on eva and styrene block polymers
CN101880517A (en) * 2010-07-19 2010-11-10 杭州天创化学技术有限公司 Low-temperature resistant hot melt glue

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Application publication date: 20181225