CN108410407A - A kind of preparation method of halogen-free flame-retardant adhesive - Google Patents
A kind of preparation method of halogen-free flame-retardant adhesive Download PDFInfo
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- CN108410407A CN108410407A CN201810353298.2A CN201810353298A CN108410407A CN 108410407 A CN108410407 A CN 108410407A CN 201810353298 A CN201810353298 A CN 201810353298A CN 108410407 A CN108410407 A CN 108410407A
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- Prior art keywords
- halogen
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- mixture
- free flame
- retardant adhesive
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Classifications
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- 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
- C09J11/04—Non-macromolecular additives inorganic
-
- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- 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
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of preparation methods of halogen-free flame-retardant adhesive, include the following steps：The preparation of S1, raw material；S2, o-phthalic acid dibutyl ester, zinc hydroxyl stannate, ferrocene are mixed with diluent, obtains mixture A, redisperse clay and talcum powder obtain mixture B；S3, by raw-silastic continuously mixing, add epoxy resin and polyurethane resin be kneaded, heat preservation, add mixture B, stir evenly up to halogen-free flame-retardant adhesive.Preparation method proposed by the present invention, easy to operate, equipment requirement is low, raw material is cheap and easy to get, it is applied widely convenient for industrialized production, the good mixing effect of each raw material, production efficiency is high, and the gluing agent prescription prepared is reasonable, the usage amount of fire retardant is few, and cementability, high temperature resistant and flame retardant property are good, not phosphorous, halogen compound, it is environmental-friendly.
Description
Technical field
The present invention relates to the preparing technical field of adhesive more particularly to a kind of preparation methods of halogen-free flame-retardant adhesive.
Background technology
Pass through the object sticked and the effects that cohesion makes two or more product or material link together at interface
Matter is referred to as adhesive, is called binder.Main application is started in the multiple fields, such as automobile such as building, industry
Machine, speed changer, vehicle bridge flat seal anaerobic adhesive etc. belong to adhesive.At present the adhesive that uses on the market in production and
Main focus is in cementability when preparation, and not high to the otherwise performance attention rate of bonding agent, causes the gluing of production
Agent is in special field in application, service life is generally partially long, for example engine will produce a large amount of heat to automobile upon actuation, lead
It is easy to aging that adhesive is obtained on cause engine, is influenced its performance, can be caused the generation of fire sometimes or even also, there are certain safety
Hidden danger.In order to improve the flame retardant property of adhesive, fire retardant would generally be added with Founder in researcher, but the fire retardant used is logical
Often contain halogen or P elements, it is caused to will produce largely the chemical combination for having pollution to environment while playing fire retardation
Object does not meet the standard of environmental protection, and the addition of fire retardant is larger, and dispersion performance is poor, causes the mixing of adhesive uniform
Degree difficulty complies with standard.Based on this, the present invention proposes a kind of preparation method of the miscible halogen-free flame-retardant adhesive of each raw material.
Invention content
The purpose of the present invention is to solve disadvantages existing in the prior art, and a kind of halogen-free flame-retardant adhesive proposed
Preparation method.
A kind of preparation method of halogen-free flame-retardant adhesive, includes the following steps：
S1, clay, talcum powder, ferrocene, zinc hydroxyl stannate, silicone coupling agents, o-phthalic acid dibutyl ester, dilution are weighed
Agent, epoxy resin, polyurethane resin and raw-silastic continuously, it is spare；
S2, the step S1 silicone coupling agents weighed are mixed with diluent, it is to be mixed uniformly after sequentially add O-phthalic
Sour dibutyl ester, zinc hydroxyl stannate and ferrocene continue to mix to uniform up to mixture A, then again as in mixture A successively dividing
Clay and talcum powder are dissipated, is uniformly dispersed up to mixture B；
S3, epoxy resin, polyurethane resin and raw-silastic continuously are weighed, and raw-silastic continuously is added in mixer and is added
Then the temperature of mixer is adjusted to 145~155 DEG C again, then epoxy resin and polyurethane resin is added to mixing by hot mixing
Machine is kneaded, and keeps the temperature 20~30min after mixing to get mixture C；
S4, the temperature for keeping mixture C in step S3, and mixture B prepared by step S2 is added, then with 500~1500r/
The speed of min stirs 15~25min, and program is cooled to room temperature up to halogen-free flame-retardant adhesive.
Preferably, the program of described program cooling is that 0~5min is cooled down with the speed of 3 DEG C/min, 5~10min with 4 DEG C/
The speed of min cools down, and 10~20min is cooled down with the speed of 5 DEG C/min, and 20~25min is cooled down with the speed of 8 DEG C/min, 25min
Cooled down later with the speed of 10 DEG C/min.
Preferably, the epoxy resin, polyurethane resin, raw-silastic continuously, clay, talcum powder, ferrocene, hydroxyl stannate
Zinc, silicone coupling agents, o-phthalic acid dibutyl ester and diluent mass ratio be 100：40~50：15~25：5~15：5~
15：0.5~1.5：1~3：0.5~1.5：0.3~0.6：30~40.
Preferably, the epoxy resin, polyurethane resin, raw-silastic continuously, clay, talcum powder, ferrocene, hydroxyl stannate
Zinc, silicone coupling agents, o-phthalic acid dibutyl ester and diluent mass ratio be 100：45：20：10：10：1：2：1：0.5：
35。
Preferably, the mass ratio of the ferrocene and zinc hydroxyl stannate is 1：1~3.
Preferably, the diluent is mixed by methanol, ethyl alcohol and acetone, and the volume ratio of methanol, ethyl alcohol and acetone
It is 1~2：3~5：1.
Compared with prior art, beneficial effects of the present invention are：
1, preparation process is easy to operate, by clay, talcum powder, ferrocene, zinc hydroxyl stannate, silicone coupling agents, O-phthalic
Sour dibutyl ester first carries out mixing with diluent can improve its rate of dispersion in major ingredient, accelerate incorporation time, improve mixing
Efficiency, and can be operated simultaneously in production, production efficiency is improved, and make the mixing uniformity of the adhesive prepared good；
2, the adhesive prepared not only has excellent cementability, while also having good high temperature resistant and flame retardant property, in turn
Expand the application range of adhesive；
3, phosphorous, halide-containing is not used in adhesive, reduces the generation of harmful substance in combustion process, it is environmentally friendly,
And the zinc hydroxyl stannate and ferrocene of rational proportion have the effect of cooperative flame retardant and suppression cigarette, reduce the dosage of fire retardant；
4, formula is reasonable, and raw material is cheap and easy to get, and manufacturing cost is low, and required equipment requirement is low, is convenient for industrialized production, the scope of application
Extensively.
Specific implementation mode
The present invention is made further to explain with reference to specific embodiment.
Embodiment one
A kind of preparation method of halogen-free flame-retardant adhesive proposed by the present invention, includes the following steps：
S1, according to epoxy resin, polyurethane resin, raw-silastic continuously, clay, talcum powder, ferrocene, zinc hydroxyl stannate, silica
The mass ratio of alkane coupling agent, o-phthalic acid dibutyl ester and diluent is 100：45：20：10：10：1：2：1：0.5：35 weigh original
Material, it is spare；
S2, the step S1 silicone coupling agents weighed are mixed with diluent, it is to be mixed uniformly after sequentially add O-phthalic
Sour dibutyl ester, zinc hydroxyl stannate and ferrocene continue to mix to uniform up to mixture A, then again as in mixture A successively dividing
Clay and talcum powder are dissipated, is uniformly dispersed up to mixture B；
S3, epoxy resin, polyurethane resin and raw-silastic continuously are weighed, and raw-silastic continuously is added in mixer and is added
Then the temperature of mixer is adjusted to 150 DEG C again, then epoxy resin and polyurethane resin is added to mixer and carried out by hot mixing
It is kneaded, keeps the temperature 25min after mixing to get mixture C；
S4, the temperature for keeping mixture C in step S3, and mixture B prepared by step S2 is added, then with 1000r/min's
Speed stirs 20min, is cooled down with the speed of 3 DEG C/min according still further to 0~5min, and 5~10min is cooled down with the speed of 4 DEG C/min, and 10
~20min is cooled down with the speed of 5 DEG C/min, and 20~25min is cooled down with the speed of 8 DEG C/min, with 10 DEG C/min's after 25min
Speed is down to room temperature up to halogen-free flame-retardant adhesive.
In the present invention, diluent is mixed by methanol, ethyl alcohol and acetone, and the volume ratio of methanol, ethyl alcohol and acetone is
1.5：4：1.
Embodiment two
A kind of preparation method of halogen-free flame-retardant adhesive proposed by the present invention, includes the following steps：
S1, according to epoxy resin, polyurethane resin, raw-silastic continuously, clay, talcum powder, ferrocene, zinc hydroxyl stannate, silica
The mass ratio of alkane coupling agent, o-phthalic acid dibutyl ester and diluent is 100：50：20：15：5：1：3：1：0.4：36 weigh original
Material, it is spare；
S2, the step S1 silicone coupling agents weighed are mixed with diluent, it is to be mixed uniformly after sequentially add O-phthalic
Sour dibutyl ester, zinc hydroxyl stannate and ferrocene continue to mix to uniform up to mixture A, then again as in mixture A successively dividing
Clay and talcum powder are dissipated, is uniformly dispersed up to mixture B；
S3, epoxy resin, polyurethane resin and raw-silastic continuously are weighed, and raw-silastic continuously is added in mixer and is added
Then the temperature of mixer is adjusted to 155 DEG C again, then epoxy resin and polyurethane resin is added to mixer and carried out by hot mixing
It is kneaded, keeps the temperature 20min after mixing to get mixture C；
S4, the temperature for keeping mixture C in step S3, and mixture B prepared by step S2 is added, then with 1500r/min's
Speed stirs 15min, is cooled down with the speed of 3 DEG C/min according still further to 0~5min, and 5~10min is cooled down with the speed of 4 DEG C/min, and 10
~20min is cooled down with the speed of 5 DEG C/min, and 20~25min is cooled down with the speed of 8 DEG C/min, with 10 DEG C/min's after 25min
Speed is down to room temperature up to halogen-free flame-retardant adhesive.
In the present invention, diluent is mixed by methanol, ethyl alcohol and acetone, and the volume ratio of methanol, ethyl alcohol and acetone is
2：5：1.
Embodiment three
A kind of preparation method of halogen-free flame-retardant adhesive proposed by the present invention, includes the following steps：
S1, according to epoxy resin, polyurethane resin, raw-silastic continuously, clay, talcum powder, ferrocene, zinc hydroxyl stannate, silica
The mass ratio of alkane coupling agent, o-phthalic acid dibutyl ester and diluent is 100：40：15：8：10：1.5：3：1.5：0.6：40 claim
Raw material is taken, it is spare；
S2, the step S1 silicone coupling agents weighed are mixed with diluent, it is to be mixed uniformly after sequentially add O-phthalic
Sour dibutyl ester, zinc hydroxyl stannate and ferrocene continue to mix to uniform up to mixture A, then again as in mixture A successively dividing
Clay and talcum powder are dissipated, is uniformly dispersed up to mixture B；
S3, epoxy resin, polyurethane resin and raw-silastic continuously are weighed, and raw-silastic continuously is added in mixer and is added
Then the temperature of mixer is adjusted to 145 DEG C again, then epoxy resin and polyurethane resin is added to mixer and carried out by hot mixing
It is kneaded, keeps the temperature 30min after mixing to get mixture C；
S4, the temperature for keeping mixture C in step S3, and mixture B prepared by step S2 is added, then with the speed of 800r/min
Degree stirring 20min is cooled down according still further to 0~5min with the speed of 3 DEG C/min, and 5~10min is cooled down with the speed of 4 DEG C/min, 10~
20min is cooled down with the speed of 5 DEG C/min, and 20~25min is cooled down with the speed of 8 DEG C/min, with the speed of 10 DEG C/min after 25min
Degree is down to room temperature up to halogen-free flame-retardant adhesive.
In the present invention, diluent is mixed by methanol, ethyl alcohol and acetone, and the volume ratio of methanol, ethyl alcohol and acetone is
2：3：1.
Comparative example one
Ferrocene equivalent in embodiment one is substituted for zinc hydroxyl stannate, other compositions are constant, the preparation process of fire retardant glue and
Parameter is also the same as embodiment one.
Comparative example two
Zinc hydroxyl stannate equivalent in embodiment one is substituted for ferrocene, other compositions are constant, the preparation process of fire retardant glue and
Parameter is also the same as embodiment one.
Fire retardant glue progressive prepared by above-described embodiment one, embodiment two, embodiment three, comparative example one and comparative example two
It can detect, it is as a result as follows：
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, and it is any
Those familiar with the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its invents
Design is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of halogen-free flame-retardant adhesive, which is characterized in that include the following steps：
S1, clay, talcum powder, ferrocene, zinc hydroxyl stannate, silicone coupling agents, o-phthalic acid dibutyl ester, dilution are weighed
Agent, epoxy resin, polyurethane resin and raw-silastic continuously, it is spare；
S2, the step S1 silicone coupling agents weighed are mixed with diluent, it is to be mixed uniformly after sequentially add O-phthalic
Sour dibutyl ester, zinc hydroxyl stannate and ferrocene continue to mix to uniform up to mixture A, then again as in mixture A successively dividing
Clay and talcum powder are dissipated, is uniformly dispersed up to mixture B；
S3, epoxy resin, polyurethane resin and raw-silastic continuously are weighed, and raw-silastic continuously is added in mixer and is added
Then the temperature of mixer is adjusted to 145~155 DEG C again, then epoxy resin and polyurethane resin is added to mixing by hot mixing
Machine is kneaded, and keeps the temperature 20~30min after mixing to get mixture C；
S4, the temperature for keeping mixture C in step S3, and mixture B prepared by step S2 is added, then with 500~1500r/
The speed of min stirs 15~25min, and program is cooled to room temperature up to halogen-free flame-retardant adhesive.
2. a kind of preparation method of halogen-free flame-retardant adhesive according to claim 1, which is characterized in that described program cools down
Program be that 0~5min is cooled down with the speed of 3 DEG C/min, 5~10min is cooled down with the speed of 4 DEG C/min, and 10~20min is with 5
DEG C/cooling of the speed of min, 20~25min cooled down with the speed of 8 DEG C/min, cooled down with the speed of 10 DEG C/min after 25min.
3. a kind of preparation method of halogen-free flame-retardant adhesive according to claim 1, which is characterized in that the asphalt mixtures modified by epoxy resin
Fat, polyurethane resin, raw-silastic continuously, clay, talcum powder, ferrocene, zinc hydroxyl stannate, silicone coupling agents, O-phthalic
The mass ratio of sour dibutyl ester and diluent is 100：40~50：15~25：5~15：5~15：0.5~1.5：1~3：0.5~
1.5：0.3~0.6：30~40.
4. a kind of preparation method of halogen-free flame-retardant adhesive according to claim 1, which is characterized in that the asphalt mixtures modified by epoxy resin
Fat, polyurethane resin, raw-silastic continuously, clay, talcum powder, ferrocene, zinc hydroxyl stannate, silicone coupling agents, O-phthalic
The mass ratio of sour dibutyl ester and diluent is 100：45：20：10：10：1：2：1：0.5：35.
5. a kind of preparation method of halogen-free flame-retardant adhesive according to claim 1, which is characterized in that the ferrocene and
The mass ratio of zinc hydroxyl stannate is 1：1~3.
6. a kind of preparation method of halogen-free flame-retardant adhesive according to claim 1, which is characterized in that the diluent by
Methanol, ethyl alcohol and acetone mix, and the volume ratio of methanol, ethyl alcohol and acetone is 1~2：3~5：1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810353298.2A CN108410407A (en) | 2018-04-19 | 2018-04-19 | A kind of preparation method of halogen-free flame-retardant adhesive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810353298.2A CN108410407A (en) | 2018-04-19 | 2018-04-19 | A kind of preparation method of halogen-free flame-retardant adhesive |
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| CN108410407A true CN108410407A (en) | 2018-08-17 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104099028A (en) * | 2014-08-04 | 2014-10-15 | 公安部四川消防研究所 | Fire-proof adhesive and application thereof |
| CN104099060A (en) * | 2013-04-03 | 2014-10-15 | 上海华硅化工新材料有限公司 | Two-composition fireproof silicone sealant |
-
2018
- 2018-04-19 CN CN201810353298.2A patent/CN108410407A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104099060A (en) * | 2013-04-03 | 2014-10-15 | 上海华硅化工新材料有限公司 | Two-composition fireproof silicone sealant |
| CN104099028A (en) * | 2014-08-04 | 2014-10-15 | 公安部四川消防研究所 | Fire-proof adhesive and application thereof |
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