CN108659718A - A kind of dedicated high viscosity sealing wax preparation method of car light - Google Patents

A kind of dedicated high viscosity sealing wax preparation method of car light Download PDF

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Publication number
CN108659718A
CN108659718A CN201810334353.3A CN201810334353A CN108659718A CN 108659718 A CN108659718 A CN 108659718A CN 201810334353 A CN201810334353 A CN 201810334353A CN 108659718 A CN108659718 A CN 108659718A
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China
Prior art keywords
parts
high viscosity
sealing wax
sulfuric acid
car light
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CN201810334353.3A
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Chinese (zh)
Inventor
时伯建
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Jiangsu New Mstar Technology Ltd
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Jiangsu New Mstar Technology Ltd
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Priority to CN201810334353.3A priority Critical patent/CN108659718A/en
Publication of CN108659718A publication Critical patent/CN108659718A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J4/00Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
    • C09J4/06Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
    • 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
    • C08G64/00Macromolecular compounds obtained by reactions forming a carbonic ester link in the main chain of the macromolecule
    • C08G64/20General preparatory processes
    • C08G64/30General preparatory processes using carbonates
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a kind of dedicated high viscosity sealing wax preparation methods of car light, belong to the preparation field of material, and the ingredient of the high viscosity sealing wax includes:Palm wax, polytrimethylene carbonate, α-cyanoacrylate, sodium metasilicate, sulfuric acid, aliphatic epoxy resin, halogenated phosphate, bonding agent, light stabilizer, polyphosphoric acid;In the method for the present invention, sulfuric acid catalysis trimethylene carbonate monomer, prepare polytrimethylene carbonate, sulfuric acid at this time continuously adds sodium metasilicate as catalyst under conditions of can not removing catalyst, sulfuric acid, sodium metasilicate reaction is allowed to prepare silica gel, maximally utilizing for component may be implemented, there are the feature for also having both high viscosity while environmentally friendly material in the sealing wax being prepared, solve defect existing for existing sealing wax.

Description

A kind of dedicated high viscosity sealing wax preparation method of car light
Technical field
The invention belongs to the preparation field of material, in particular to a kind of dedicated high viscosity sealing wax preparation methods of car light.
Background technology
With the development of automobile industry, the accessory and dispensing etc. that are related in automobile are also required to develop therewith.Wherein car light The sealing wax of position-specific is also required to develop therewith, wherein the characteristic for needing most developmental research is stickiness speciality, due in vehicle The problem of lamp position is set, therefore sealing wax will also be by relatively-high temperature and illumination.There is also not environmentally for sealing wax on the market Characteristic, therefore while have high viscosity, it is to be prepared to be also equipped with environmentally friendly car light Special seal wax strategic point.
Invention content
The present invention is directed to problems of the prior art, and the invention discloses a kind of dedicated high viscosity sealing waxs of car light The ep-type material of polytrimethylene carbonate is added in the case of selecting palm wax as basic substance in preparation method, with And the cooperation of other a series of components, car light Special seal wax that is environmentally friendly and having high viscosity is finally prepared.
The invention is realized in this way:
A kind of dedicated high viscosity sealing wax of car light, which is characterized in that the ingredient of the sealing wax includes:
It is palm wax, polytrimethylene carbonate, α-cyanoacrylate, sodium metasilicate, sulfuric acid, aliphatic epoxy resin, halogenated Phosphate, bonding agent, light stabilizer, polyphosphoric acid;
It is in terms of 100 parts by the quality of palm wax;
The quality of polytrimethylene carbonate be 30 ~ 100 parts, 1 ~ 2 part of α-cyanoacrylate, 20 ~ 30 parts of sodium metasilicate, sulphur 1 ~ 2 part of acid, 5 ~ 10 parts of halogenated phosphate, 5 ~ 10 parts of bonding agent, 1 ~ 2 part of light stabilizer, gathers 10 ~ 20 parts of aliphatic epoxy resin 3 ~ 5 parts of phosphoric acid.
Further, the degree of polymerization of the polytrimethylene carbonate is 30 ~ 100.
Further, the bonding agent is PP bonding agents.
Further, the light stabilizer is hindered amine light stabilizer.
The invention also discloses a kind of preparation methods of the dedicated high viscosity sealing wax of car light, and steps are as follows:
Step 1:The preparation of polytrimethylene carbonate;It is 30 ~ 100 to take the mass parts of trimethylene carbonate monomer, takes sulfuric acid 1 ~ 2 part, after reacting 5 ~ 20 hours, polytrimethylene carbonate is prepared;
Step 2:Based on the mixture of the polytrimethylene carbonate in step 1, reaction is not terminated, sodium metasilicate is added wherein 20 ~ 30 parts, polytrimethylene is prepared in the sulfuric acid reaction in the mixture of sodium metasilicate and polytrimethylene carbonate at this time The composition of carbonic ester and silica gel, the sulfuric acid catalyst for not terminating reaction do not need to be precipitated at this time, but directly and silicic acid Sodium reaction prepares silica gel content;
Step 3:100 parts of palm wax, 10 ~ 20 parts of aliphatic epoxy resin, halophosphoric acid are added in the composition of step 2 Ester, at ambient temperature by agitating device be uniformly mixed, until polytrimethylene carbonate powdered substance disappear in it is mixed It closes in object;
Step 4:It is steady that 1 ~ 2 part of α-cyanoacrylate, 5 ~ 10 parts of bonding agent, light are eventually adding in the mixture of step 3 Determine 1 ~ 2 part of agent, 3 ~ 5 parts of polyphosphoric acid, be uniformly mixed in 40 ~ 50 DEG C of temperature, uniformly after be down to room temperature, the mixing of high temperature can be with So that being mixed between substance more uniformly.
Further, trimethylene carbonate monomer and sulfuric acid are reacted in dichloromethane or ontology in the step one Reaction.
Further, reaction in methylene chloride, temperature are 25 ± 3 DEG C;Reaction in ontology is 100 ± 10 DEG C.
Further, it when the trimethylene carbonate monomer reacts in methylene chloride with sulfuric acid, after the completion of reaction, waits for Next step is carried out after dichloromethane volatilization, bulk reaction is due to being not need to dichloromethane under conditions of non-solvent The volatilisation step of alkane.
The advantageous effect of the present invention and the prior art is:
1)Polytrimethylene carbonate is the polymer of environment-friendly type, has certain elasticity, in the mixture formed with silica gel In still have the characteristic of transparence, suitable for the concrete application of car light;
2)The positive good utilisation sulfuric acid catalysis trimethylene carbonate monomer in preparation method prepares polytrimethylene carbonate, this When sulfuric acid continuously add sodium metasilicate under conditions of can not removing catalyst as catalyst, allow sulfuric acid, sodium metasilicate reaction Silica gel is prepared, maximally utilizing for component may be implemented;
3)Halogenated phosphate, polyphosphoric acid are added in component, the sealing wax under conditions of direct projection of car light can be alleviated and become xanthochromia It is black, to influence the use of car light;
4)After α-cyanoacrylate is added, sealing wax of the invention when in use, not only has the characteristic of high viscosity, together When can also shorten sealing time for playing a role of was moulding.
Specific implementation mode
It is clear to keep the purpose of the present invention, technical solution and effect clearer, example is exemplified below to the present invention into one Step is described in detail.It should be understood that specific implementation described herein is not intended to limit the present invention only to explain the present invention.
Embodiment 1
Step 1:The preparation of polytrimethylene carbonate;It is 30 parts to take the mass parts of trimethylene carbonate monomer, takes sulfuric acid 1 Part, 25 ± 3 DEG C in dichloromethane solvent, after reacting 5 hours, polytrimethylene carbonate is prepared;
Step 2:Based on the mixture of the polytrimethylene carbonate in step 1, volatilizees after dichloromethane, does not terminate reaction, 20 parts of sodium metasilicate is added wherein, prepared by the sulfuric acid reaction in the mixture of sodium metasilicate and polytrimethylene carbonate at this time Obtain the composition of polytrimethylene carbonate and silica gel;
Step 3:100 parts of palm wax, 10 parts of aliphatic epoxy resin, halogenated phosphate 5 are added in the composition of step 2 Part, at ambient temperature by agitating device be uniformly mixed, until polytrimethylene carbonate powdered substance disappear in it is mixed It closes in object;
Step 4:1 part of α-cyanoacrylate, 5 parts of PP bonding agents, hindered amine are eventually adding in the mixture of step 3 1 part of light stabilizer, 3 parts of polyphosphoric acid are uniformly mixed in 40 ~ 50 DEG C of temperature, uniformly after be down to room temperature that car light is prepared be special High viscosity sealing wax.
Embodiment 2
Step 1:The preparation of polytrimethylene carbonate;It is 50 to take the mass parts of trimethylene carbonate monomer, takes sulfuric acid 1.5 Part, bulk reaction, the reaction in ontology is 100 ± 10 DEG C, and after reaction 10 hours, polytrimethylene carbonate is prepared;
Step 2:Based on the mixture of the polytrimethylene carbonate in step 1, reaction is not terminated, sodium metasilicate is added wherein 25 parts, polytrimethylene carbon is prepared in the sulfuric acid reaction in the mixture of sodium metasilicate and polytrimethylene carbonate at this time The composition of acid esters and silica gel;
Step 3:100 parts of palm wax, 15 parts of aliphatic epoxy resin, halogenated phosphate 10 are added in the composition of step 2 Part, at ambient temperature by agitating device be uniformly mixed, until polytrimethylene carbonate powdered substance disappear in it is mixed It closes in object;
Step 4:2 parts of α-cyanoacrylate, 10 parts of PP bonding agents, hindered amine are eventually adding in the mixture of step 3 2 parts of light stabilizer, 5 parts of polyphosphoric acid are uniformly mixed in 40 ~ 50 DEG C of temperature, uniformly after be down to room temperature that car light is prepared be special High viscosity sealing wax.
Embodiment 3
Step 1:The preparation of polytrimethylene carbonate;It is 50 parts to take the mass parts of trimethylene carbonate monomer, takes sulfuric acid 1.3 parts, 25 ± 3 DEG C in dichloromethane solvent, after reacting 8 hours, polytrimethylene carbonate is prepared;
Step 2:Based on the mixture of the polytrimethylene carbonate in step 1, volatilizees after dichloromethane, does not terminate reaction, 30 parts of sodium metasilicate is added wherein, prepared by the sulfuric acid reaction in the mixture of sodium metasilicate and polytrimethylene carbonate at this time Obtain the composition of polytrimethylene carbonate and silica gel;
Step 3:100 parts of palm wax, 15 parts of aliphatic epoxy resin, halogenated phosphate 7 are added in the composition of step 2 Part, at ambient temperature by agitating device be uniformly mixed, until polytrimethylene carbonate powdered substance disappear in it is mixed It closes in object;
Step 4:1 part of α-cyanoacrylate, 7 parts of PP bonding agents, hindered amine are eventually adding in the mixture of step 3 1 part of light stabilizer, 4 parts of polyphosphoric acid are uniformly mixed in 40 ~ 50 DEG C of temperature, uniformly after be down to room temperature that car light is prepared be special High viscosity sealing wax.
Embodiment 4
Step 1:The preparation of polytrimethylene carbonate;It is 90 to take the mass parts of trimethylene carbonate monomer, takes sulfuric acid 1.8 Part, bulk reaction, the reaction in ontology is 100 ± 10 DEG C, and after reaction 20 hours, polytrimethylene carbonate is prepared;
Step 2:Based on the mixture of the polytrimethylene carbonate in step 1, reaction is not terminated, sodium metasilicate is added wherein 30 parts, polytrimethylene carbon is prepared in the sulfuric acid reaction in the mixture of sodium metasilicate and polytrimethylene carbonate at this time The composition of acid esters and silica gel;
Step 3:100 parts of palm wax, 18 parts of aliphatic epoxy resin, halogenated phosphate 9 are added in the composition of step 2 Part, at ambient temperature by agitating device be uniformly mixed, until polytrimethylene carbonate powdered substance disappear in it is mixed It closes in object;
Step 4:2 parts of α-cyanoacrylate, 9 parts of PP bonding agents, hindered amine are eventually adding in the mixture of step 3 2 parts of light stabilizer, 4 parts of polyphosphoric acid are uniformly mixed in 40 ~ 50 DEG C of temperature, uniformly after be down to room temperature that car light is prepared be special High viscosity sealing wax.
Embodiment 5
Step 1:The preparation of polytrimethylene carbonate;It is 100 to take the mass parts of trimethylene carbonate monomer, takes sulfuric acid 2 Part, 25 ± 3 DEG C in dichloromethane solvent, after reacting 10 hours, polytrimethylene carbonate is prepared;
Step 2:Based on the mixture of the polytrimethylene carbonate in step 1, volatilizees after dichloromethane, does not terminate reaction, 30 parts of sodium metasilicate is added wherein, prepared by the sulfuric acid reaction in the mixture of sodium metasilicate and polytrimethylene carbonate at this time Obtain the composition of polytrimethylene carbonate and silica gel;
Step 3:100 parts of palm wax, 20 parts of aliphatic epoxy resin, halogenated phosphate 7 are added in the composition of step 2 Part, at ambient temperature by agitating device be uniformly mixed, until polytrimethylene carbonate powdered substance disappear in it is mixed It closes in object;
Step 4:2 parts of α-cyanoacrylate, 6 parts of PP bonding agents, hindered amine are eventually adding in the mixture of step 3 2 parts of light stabilizer, 5 parts of polyphosphoric acid are uniformly mixed in 40 ~ 50 DEG C of temperature, uniformly after be down to room temperature that car light is prepared be special High viscosity sealing wax.
Embodiment 6
Step 1:The preparation of polytrimethylene carbonate;It is 70 to take the mass parts of trimethylene carbonate monomer, takes 1 part of sulfuric acid, 25 ± 3 DEG C in dichloromethane solvent, after reacting 9 hours, polytrimethylene carbonate is prepared;
Step 2:Based on the mixture of the polytrimethylene carbonate in step 1, volatilizees after dichloromethane, does not terminate reaction, 28 parts of sodium metasilicate is added wherein, prepared by the sulfuric acid reaction in the mixture of sodium metasilicate and polytrimethylene carbonate at this time Obtain the composition of polytrimethylene carbonate and silica gel;
Step 3:100 parts of palm wax, 16 parts of aliphatic epoxy resin, halogenated phosphate 6 are added in the composition of step 2 Part, at ambient temperature by agitating device be uniformly mixed, until polytrimethylene carbonate powdered substance disappear in it is mixed It closes in object;
Step 4:1 part of α-cyanoacrylate, 6 parts of PP bonding agents, hindered amine are eventually adding in the mixture of step 3 2 parts of light stabilizer, 3 parts of polyphosphoric acid are uniformly mixed in 40 ~ 50 DEG C of temperature, uniformly after be down to room temperature that car light is prepared be special High viscosity sealing wax.

Claims (8)

1. a kind of dedicated high viscosity sealing wax of car light, which is characterized in that the ingredient of the sealing wax includes:
It is palm wax, polytrimethylene carbonate, α-cyanoacrylate, sodium metasilicate, sulfuric acid, aliphatic epoxy resin, halogenated Phosphate, bonding agent, light stabilizer, polyphosphoric acid;
It is in terms of 100 parts by the quality of palm wax;
The quality of polytrimethylene carbonate be 30 ~ 100 parts, 1 ~ 2 part of α-cyanoacrylate, 20 ~ 30 parts of sodium metasilicate, sulphur 1 ~ 2 part of acid, 5 ~ 10 parts of halogenated phosphate, 5 ~ 10 parts of bonding agent, 1 ~ 2 part of light stabilizer, gathers 10 ~ 20 parts of aliphatic epoxy resin 3 ~ 5 parts of phosphoric acid.
2. the dedicated high viscosity sealing wax of a kind of car light according to claim 1, which is characterized in that poly- three methylene The degree of polymerization of base carbonic ester is 30 ~ 100.
3. the dedicated high viscosity sealing wax of a kind of car light according to claim 1, which is characterized in that the bonding agent is PP bonding agents.
4. the dedicated high viscosity sealing wax of a kind of car light according to claim 1, which is characterized in that the light stabilizer For hindered amine light stabilizer.
5. according to a kind of preparation method of the dedicated high viscosity sealing wax of car light described in claim 1 ~ 4, which is characterized in that step It is rapid as follows:
Step 1:The preparation of polytrimethylene carbonate;It is 30 ~ 100 to take the mass parts of trimethylene carbonate monomer, takes sulfuric acid 1 ~ 2 part, after reacting 5 ~ 20 hours, polytrimethylene carbonate is prepared;
Step 2:Based on the mixture of the polytrimethylene carbonate in step 1, reaction is not terminated, sodium metasilicate is added wherein 20 ~ 30 parts, polytrimethylene is prepared in the sulfuric acid reaction in the mixture of sodium metasilicate and polytrimethylene carbonate at this time The composition of carbonic ester and silica gel;
Step 3:100 parts of palm wax, 10 ~ 20 parts of aliphatic epoxy resin, halophosphoric acid are added in the composition of step 2 Ester, at ambient temperature by agitating device be uniformly mixed, until polytrimethylene carbonate powdered substance disappear in it is mixed It closes in object;
Step 4:It is steady that 1 ~ 2 part of α-cyanoacrylate, 5 ~ 10 parts of bonding agent, light are eventually adding in the mixture of step 3 Determine 1 ~ 2 part of agent, 3 ~ 5 parts of polyphosphoric acid, be uniformly mixed in 40 ~ 50 DEG C of temperature, room temperature is down to after uniform.
6. a kind of preparation method of the dedicated high viscosity sealing wax of car light according to claim 5, which is characterized in that described The step of one in trimethylene carbonate monomer and sulfuric acid react in dichloromethane or bulk reaction.
7. a kind of preparation method of the dedicated high viscosity sealing wax of car light according to claim 6, which is characterized in that two Reaction in chloromethanes, temperature are 25 ± 3 DEG C;Reaction in ontology is 100 ± 10 DEG C.
8. according to a kind of preparation method of any dedicated high viscosity sealing wax of car light of claim 6 ~ 7, feature exists In, when the trimethylene carbonate monomer reacts in methylene chloride with sulfuric acid, after the completion of reaction, wait for dichloromethane volatilize After carry out next step.
CN201810334353.3A 2018-04-14 2018-04-14 A kind of dedicated high viscosity sealing wax preparation method of car light Pending CN108659718A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101864259A (en) * 2010-05-05 2010-10-20 广州市豪特粘接材料有限公司 SIS (Styrene-Isoprene-Styrene) hot melt adhesive for car light adhesion and preparation method thereof
CN101878245A (en) * 2007-11-30 2010-11-03 纳幕尔杜邦公司 Process to make a poly(trimethylene carbonate) glycol
CN107090262A (en) * 2017-06-19 2017-08-25 上海都伟光伏科技有限公司 A kind of good composition epoxy resin of transparency and its applied in automotive field
WO2017170079A1 (en) * 2016-04-01 2017-10-05 国立大学法人東京農工大学 Pyrolytic binder

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101878245A (en) * 2007-11-30 2010-11-03 纳幕尔杜邦公司 Process to make a poly(trimethylene carbonate) glycol
CN101864259A (en) * 2010-05-05 2010-10-20 广州市豪特粘接材料有限公司 SIS (Styrene-Isoprene-Styrene) hot melt adhesive for car light adhesion and preparation method thereof
WO2017170079A1 (en) * 2016-04-01 2017-10-05 国立大学法人東京農工大学 Pyrolytic binder
CN107090262A (en) * 2017-06-19 2017-08-25 上海都伟光伏科技有限公司 A kind of good composition epoxy resin of transparency and its applied in automotive field

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