CN104845579B - A kind of preparation method of vehicle glass glass cement - Google Patents
A kind of preparation method of vehicle glass glass cement Download PDFInfo
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- CN104845579B CN104845579B CN201510240301.6A CN201510240301A CN104845579B CN 104845579 B CN104845579 B CN 104845579B CN 201510240301 A CN201510240301 A CN 201510240301A CN 104845579 B CN104845579 B CN 104845579B
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Abstract
The invention discloses a kind of preparation method of vehicle glass glass cement, which is made of component A and B component, and component A and B component weight part ratio are 1: 3-5；Wherein, component A is that base polyurethane prepolymer for use as I and base polyurethane prepolymer for use as II is formed, and wherein the weight ratio of base polyurethane prepolymer for use as I and base polyurethane prepolymer for use as II are 1-2: 1；B component is made of following raw materials according in parts by weight: polyether polyol, light calcium, coarse whiting, nano-TiO2Powder, -200 mesh SiC powder, plasticizer, catalyst, thixotropic agent；The preparation method is that: 1) mix component A；2) filler in B component is mixed；3) component A of step 1) is added in the container with blender, then the filler mixture of step 2) preparation is added, blender revolving speed is about 500-600r/min, and stir about 40-60 minutes, polyether polyol, plasticizer, catalyst, thixotropic agent is then added；4) improve mixing speed to 700-800r/min, after stirring 60-90 minute, progress deaeration to get.
Description
Technical field
The present invention relates to sealing material field, in particular to a kind of preparation method of vehicle glass glass cement.
Background technique
Glass cement is for filling gap (hole, connector, seam etc.) and having the material of bonding effect to filling base interface
Material, specifically includes that organosilicon (including modified organic silicon) class, polyurethanes, polysulfide rubber class, esters of acrylic acid, SBR rubber
Class, butyl type rubber, pitch, oiliness filleting glue class etc..And it is used to fill to have caused by must being subjected to vibration or rising-heat contracting-cold etc. and stretch
The gap of contracting must then use spring glass glue.Spring glass glue is will to be bonded and seal the production that two kinds of functions roll into one
Product.Wherein the three classes top grade spring glass glue of better performances is silicone glass glue, polysulfide glass cement and polyurethane glass respectively
Glue.In recent years, application of the spring glass glue in much industry such as building, building, automobile, ship, electrical communications, civil field
It is more and more extensive.
In above-mentioned spring glass glue, polyurethane glass glue is with the fastest developing speed, and demand is gradually increased, and is because it has
Excellent performance.The characteristics of polyurethane glass glue, has: (1) excellent wearability；(2) low-temperature pliability；(3) model is adjusted in performance
It encloses wide；(4) mechanical strength is big；(5) cementability is good；(6) elasticity is good, has excellent restoration, is suitably adapted for dynamic juncture；(7)
Good weatherability, service life are 15-20；(8) oil resistivity is excellent；(9) resistance to biological aging；(10) moderate.
The existing polyurethane glass glue especially existing defect when vehicle glass is installed: mono-component polyurethane glass cement is used
When vehicle glass is assembled and is bonded, bulk strength is lower than 450% (GB/T528) lower than 8Mpa (GB/T528) or elongation percentage.②
At such as 0 DEG C -10 DEG C of low temperature, solidification rate is lower than 3.0mm/24 hours (10 DEG C ± 2 DEG C, 30% ± 5% humidity).Drawbacks described above
Affect the application effect or effect of mono-component polyurethane glass cement.
Patent document CN200810043539.X discloses a kind of polyurethane sealant, and disclosing it is two-component, gram
The segmental defect of one-component colloid is taken, but the patent, there is no its colloid technology index is disclosed, through practical proof, mechanics refers to
Mark, room temperature and low temperature curing properties are not able to satisfy the requirement of vehicle glass still.
Summary of the invention
In view of the deficiencies of the prior art, one of the objects of the present invention is to provide a kind of preparations of vehicle glass glass cement
The glass cement of method, this method preparation improves bulk strength and elongation percentage, and has high solidification rate at low temperature, overcomes existing
Mono-component polyurethane glass cement existing for defect.
To achieve the above object, the present invention adopts the following technical scheme that:
A kind of preparation method of vehicle glass glass cement, the glass cement are made of component A and B component, component A and B group
Dividing weight part ratio is 1: 3-5；Wherein, component A is that base polyurethane prepolymer for use as I and base polyurethane prepolymer for use as II is formed, and wherein polyurethane is pre-
Aggressiveness I is end alkoxysilane group base polyurethane prepolymer for use as, and base polyurethane prepolymer for use as II is made by following methods: by biuret polyisocyanate cyanogen
Acid esters, which is reacted with polyether polyol at 105-110 DEG C, to be made, wherein the mass ratio of biuret polyisocyanate and polyether polyol
It is 28-30: 1, wherein the weight ratio of base polyurethane prepolymer for use as I and base polyurethane prepolymer for use as II are 1-2: 1；B component is by with weight
The following raw materials according composition of part meter: 44-48 parts of polyether polyol；18-22 parts of light calcium, 25-27 parts of coarse whiting, nano-TiO2Powder 4-6
Part, -200 4-6 parts of mesh SiC powder, 17-19 parts of plasticizer；0.1-0.3 parts of catalyst；0.1-0.3 parts of thixotropic agent；The preparation side
Method are as follows:
1) it mixes component A: selecting commercially available end alkoxysilane group base polyurethane prepolymer for use as, then prepare poly- ammonia according to the above method
Ester performed polymer II, then two kinds of components are uniformly mixed by weight ratio；
2) filler in B component is mixed: by light calcium, coarse whiting, the nano-TiO in B component2Powder, -200 mesh SiC powder are common
It is pre-mixed in batch mixer about 150-180 minutes, obtains filler mixture；
3) component A of step 1) is added in the container with blender, the filler mixture of step 2) preparation is then added,
Blender revolving speed is about 500-600r/min, stir about 40-60 minutes, be then added polyether polyol, plasticizer, catalyst,
Thixotropic agent；
4) improve mixing speed to 700-800r/min, after stirring 60-90 minute, progress deaeration to get.Wherein, described
Polyether polyol is selected from polyoxypropylene polyol, polymer polyatomic alcohol, polytetrahydrofuran, polyethylene glycol oxide.
Wherein, the plasticizer is selected from phthalic acid rouge, aliphatic diacid rouge, phosphate ester, two alcohol ester of benzoic acid.
Wherein, the catalyst is selected from dibutyl tin dilaurate, lead octoate, stannous octoate, tertiary amines, wherein it is preferred that two
Dibutyl tin laurate or stannous octoate.
Wherein, the thixotropic agent is selected from gas-phase silica, rilanit special, polyamide or bentonite.
The performance of glass cement greatly improved by having carried out following improvement to the prior art in the present invention, obtains beneficial
Technical effect:
1) preferred two kinds of base polyurethane prepolymer for use as are chosen, and its mixed proportion has been determined；
2) optimization filler composition, including following aspect: a. selects component: determining light calcium, coarse whiting, nano-TiO2Powder and
SiC is as filler；B. determine content: 18-22 parts of light calcium, 25-27 parts of coarse whiting, nano-TiO24-6 parts of powder, -200 mesh SiC powder 4-6
Part；C. it determines granularity, including uses nano-TiO2Powder, and limit the granularity of SiC as -200 mesh, wherein nano-TiO2Powder especially selects
The emphasis selected, usual micron order TiO2Powder plays the role of as pigment (titanium dioxide) or filler it is well known that but addition nanometer
TiO2After powder, there is pole significantly to be promoted performance, surmounted the scope of pigment and filler, to the synthesis of entire glass cement
Performance has played important influence.Experiment shows that the selection of said components, the determination of content and the selection of granularity have mutually association
The application, which is not achieved, in the interactively of tune, increase other components or the variation for reducing certain component, content and granularity to reach
The performance indicator arrived.
3) inorganic powdered filler is first carried out mixing dispersion by preparation method of the invention, then carries out the preparation of glass cement, is made
The glass cement performance stable homogeneous that must be prepared, to ensure that preferable mechanical property.
Glass cement of the invention has following performance characteristics:
1) it is tested by GB/T528, tensile strength after the glass adhesive curing is 12.2-14.0MPa, and its elongation at break
For 470-520%；Therefore, excellent in mechanical performance.
2) the polyurethane glass glue has preferable solidification not only under 15 DEG C -30 DEG C of room temperature, 50 ± 5% humidity environments
Rate, such as larger than 8mm/24 hour, while under the conditions of low temperature (0 DEG C -15 DEG C) and low humidity (30 ± 5% humidity), also have very high
Solidification rate, be greater than 5.5mm/24 hours.
Specific embodiment
Embodiment one
A kind of preparation method of vehicle glass glass cement, the glass cement are made of component A and B component, component A and B group
Dividing weight part ratio is 1: 3；Wherein, component A is that base polyurethane prepolymer for use as I and base polyurethane prepolymer for use as II is formed, wherein polyurethane prepolymer
Body I is end alkoxysilane group base polyurethane prepolymer for use as, and base polyurethane prepolymer for use as II is made by following methods: by biuret polyisocyanic acid
Ester, which is reacted with polyether polyol at 105 DEG C, to be made, and wherein biuret polyisocyanate and the mass ratio of polyether polyol are 28: 1,
Wherein the weight ratio of base polyurethane prepolymer for use as I and base polyurethane prepolymer for use as II are 1: 1；B component is by following original in parts by weight
Material composition: 44 parts of polytetrahydrofuran；22 parts of light calcium, 25 parts of coarse whiting, nano-TiO26 parts of powder, -200 4 parts of mesh SiC powder, O-phthalic
19 parts of sour rouge；0.1 part of dibutyl tin dilaurate；0.3 part of gas-phase silica；The preparation method is that:
1) it mixes component A: selecting commercially available end alkoxysilane group base polyurethane prepolymer for use as, then prepare poly- ammonia according to the above method
Ester performed polymer II, then two kinds of components are uniformly mixed by weight ratio；
2) filler in B component is mixed: by light calcium, coarse whiting, the nano-TiO in B component2Powder, -200 mesh SiC powder are common
It is pre-mixed in batch mixer about 150 minutes, obtains filler mixture；
3) component A of step 1) is added in the container with blender, the filler mixture of step 2) preparation is then added,
Blender revolving speed is about 600r/min, and stir about 40 minutes, polytetrahydrofuran, phthalic acid rouge, tin dilaurate is then added
Dibutyl tin, gas-phase silica；
4) improve mixing speed to 700r/min, after stirring 90 minutes, carry out deaeration to get.
It is tested by GB/T528, the tensile strength after the glass adhesive curing is 13.4MPa, and its elongation at break is
490%；For the polyurethane glass glue under 15 DEG C -30 DEG C of room temperature, 50 ± 5% humidity environments, it is small that solidification rate is greater than 8mm/24
When, while under the conditions of low temperature (0 DEG C -15 DEG C) and low humidity (30 ± 5% humidity), solidification rate is greater than 5.5mm/24 hours.
Embodiment two
A kind of preparation method of vehicle glass glass cement, the glass cement are made of component A and B component, component A and B group
Dividing weight part ratio is 1: 5；Wherein, component A is that base polyurethane prepolymer for use as I and base polyurethane prepolymer for use as II is formed, wherein polyurethane prepolymer
Body I is end alkoxysilane group base polyurethane prepolymer for use as, and base polyurethane prepolymer for use as II is made by following methods: by biuret polyisocyanic acid
Ester, which is reacted with polyether polyol at 110 DEG C, to be made, and wherein biuret polyisocyanate and the mass ratio of polyether polyol are 30: 1,
Wherein the weight ratio of base polyurethane prepolymer for use as I and base polyurethane prepolymer for use as II are 2: 1；B component is by following original in parts by weight
Material composition: 48 parts of polytetrahydrofuran；18 parts of light calcium, 27 parts of coarse whiting, nano-TiO24 parts of powder, -200 6 parts of mesh SiC powder, O-phthalic
17 parts of sour rouge；0.3 part of dibutyl tin dilaurate；0.1 part of gas-phase silica；The preparation method is that:
1) it mixes component A: selecting commercially available end alkoxysilane group base polyurethane prepolymer for use as, then prepare poly- ammonia according to the above method
Ester performed polymer II, then two kinds of components are uniformly mixed by weight ratio；
2) filler in B component is mixed: by light calcium, coarse whiting, the nano-TiO in B component2Powder, -200 mesh SiC powder are common
It is pre-mixed in batch mixer about 150-180 minutes, obtains filler mixture；
3) component A of step 1) is added in the container with blender, the filler mixture of step 2) preparation is then added,
Blender revolving speed is about 600r/min, and stir about 40 minutes, polytetrahydrofuran, phthalic acid rouge, tin dilaurate is then added
Dibutyl tin, gas-phase silica；
4) improve mixing speed to 800r/min, stirring after sixty minutes, carry out deaeration to get.
It is tested by GB/T528, the tensile strength after the glass adhesive curing is 12.4MPa, and its elongation at break is
500%；For the polyurethane glass glue under 15 DEG C -30 DEG C of room temperature, 50 ± 5% humidity environments, solidification rate is greater than 8.3mm/24
Hour, while under the conditions of low temperature (0 DEG C -15 DEG C) and low humidity (30 ± 5% humidity), solidification rate is greater than 6mm/24 hours.
Embodiment three
A kind of preparation method of vehicle glass glass cement, the glass cement are made of component A and B component, component A and B group
Dividing weight part ratio is 1: 4；Wherein, component A is that base polyurethane prepolymer for use as I and base polyurethane prepolymer for use as II is formed, wherein polyurethane prepolymer
Body I is end alkoxysilane group base polyurethane prepolymer for use as, and base polyurethane prepolymer for use as II is made by following methods: by biuret polyisocyanic acid
Ester, which is reacted with polyether polyol at 110 DEG C, to be made, and wherein biuret polyisocyanate and the mass ratio of polyether polyol are 29: 1,
Wherein the weight ratio of base polyurethane prepolymer for use as I and base polyurethane prepolymer for use as II are 1.5: 1；B component is following by parts by weight
Raw material composition: 46 parts of polyethylene glycol oxide；20 parts of light calcium, 26 parts of coarse whiting, nano-TiO25 parts of powder, -200 5 parts of mesh SiC powder, aliphatic
18 parts of diacid rouge；0.2 part of stannous octoate；0.2 part of polyamide；The preparation method is that:
1) it mixes component A: selecting commercially available end alkoxysilane group base polyurethane prepolymer for use as, then prepare poly- ammonia according to the above method
Ester performed polymer II, then two kinds of components are uniformly mixed by weight ratio；
2) filler in B component is mixed: by light calcium, coarse whiting, the nano-TiO in B component2Powder, -200 mesh SiC powder are common
It is pre-mixed in batch mixer about 165 minutes, obtains filler mixture；
3) component A of step 1) is added in the container with blender, the filler mixture of step 2) preparation is then added,
Blender revolving speed is about 550r/min, stir about 50 minutes, be then added polyethylene glycol oxide, aliphatic diacid rouge, stannous octoate,
Polyamide；
4) improve mixing speed to 750r/min, after stirring 75 minutes, carry out deaeration to get.
It is tested by GB/T528, the tensile strength after the glass adhesive curing is 13.8MPa, and its elongation at break is
520%；For the polyurethane glass glue under 15 DEG C -30 DEG C of room temperature, 50 ± 5% humidity environments, it is small that solidification rate is greater than 9mm/24
When, while under the conditions of low temperature (0 DEG C -15 DEG C) and low humidity (30 ± 5% humidity), solidification rate is greater than 6mm/24 hours.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (5)
1. a kind of preparation method of vehicle glass glass cement, which is characterized in that the glass cement is made of component A and B component, A
Component and B component weight part ratio are 1: 3-5；Wherein, component A forms for base polyurethane prepolymer for use as I and base polyurethane prepolymer for use as II, wherein
Base polyurethane prepolymer for use as I is end alkoxysilane group base polyurethane prepolymer for use as, and base polyurethane prepolymer for use as II is made by following methods: will contract two
Urea polyisocyanates, which is reacted with polyether polyol at 105-110 DEG C, to be made, wherein biuret polyisocyanate and polyether polyol
Mass ratio be 28-30:1, wherein the weight ratio of base polyurethane prepolymer for use as I and base polyurethane prepolymer for use as II be 1-2:1；B component
It is made of following raw materials according in parts by weight: 44-48 parts of polyether polyol；18-22 parts of light calcium, 25-27 parts of coarse whiting, nano-TiO2
4-6 parts of powder, -200 4-6 parts of mesh SiC powder, 17-19 parts of plasticizer；0.1-0.3 parts of catalyst；0.1-0.3 parts of thixotropic agent；The system
Preparation Method are as follows:
1) it mixes component A: selecting commercially available end alkoxysilane group base polyurethane prepolymer for use as, it is pre- then to prepare polyurethane according to the above method
Aggressiveness II, then two kinds of components are uniformly mixed by weight ratio；
2) filler in B component is mixed: by light calcium, coarse whiting, the nano-TiO in B component2Powder, -200 mesh SiC powder are in common mixing
It carries out being pre-mixed 150-180 minutes in machine, obtains filler mixture；
3) component A of step 1) is added in the container with blender, the filler mixture of step 2 preparation, stirring is then added
Machine revolving speed is 500-600r/min, stirs 40-60 minutes, polyether polyol, plasticizer, catalyst, thixotropic agent is then added；
4) improve mixing speed to 700-800r/min, after stirring 60-90 minute, progress deaeration to get;
Tensile strength after the glass adhesive curing is 12.2-14.0MPa, and its elongation at break is 470-520%；Simultaneously 0
Under DEG C -15 DEG C of low temperature and 30 ± 5% damp condition, solidification rate is greater than 5.5mm/24 hours.
2. a kind of preparation method of vehicle glass glass cement as described in claim 1, which is characterized in that the polyether polyols
Alcohol is selected from polyoxypropylene polyol, polymer polyatomic alcohol, polytetrahydrofuran, polyethylene glycol oxide.
3. a kind of preparation method of vehicle glass glass cement as described in claim 1, which is characterized in that the plasticizer choosing
From phthalic acid ester, aliphatic diacid ester, phosphate, glycol benzoate.
4. a kind of preparation method of vehicle glass glass cement as described in claim 1, which is characterized in that the catalyst choosing
From dibutyl tin dilaurate or stannous octoate.
5. a kind of preparation method of vehicle glass glass cement as described in claim 1, which is characterized in that the thixotropic agent choosing
From gas-phase silica, rilanit special, polyamide or bentonite.
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| CN107987773A (en) * | 2017-12-19 | 2018-05-04 | 上海德联化工有限公司 | A kind of automobile using composite polyurethane glass cement and preparation method thereof |
| GB202003628D0 (en) | 2020-03-12 | 2020-04-29 | Pilkington Group Ltd | Vehicle windscreen assembly |
| CN112375200A (en) * | 2020-11-13 | 2021-02-19 | 广东盛业化学科技有限公司 | Low-temperature low-humidity fast-curing polyurethane composition and preparation method thereof |
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| CN101613587B (en) * | 2008-06-24 | 2012-04-18 | 上海天补建筑科技有限公司 | Polyurethane sealing glue |
| CN103834345B (en) * | 2012-11-22 | 2017-05-31 | 湖北回天新材料股份有限公司 | A kind of excellent one-component damp solidifying polyurethane fluid sealant of UV resistant performance |
| CN104531040A (en) * | 2014-10-09 | 2015-04-22 | 广东新展化工新材料有限公司 | Polyurethane acrylate sealant and preparation method thereof |
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