CN107903665A - A kind of silicone adhesive modified zeolite powder, preparation method thereof - Google Patents
A kind of silicone adhesive modified zeolite powder, preparation method thereof Download PDFInfo
- Publication number
- CN107903665A CN107903665A CN201711217985.3A CN201711217985A CN107903665A CN 107903665 A CN107903665 A CN 107903665A CN 201711217985 A CN201711217985 A CN 201711217985A CN 107903665 A CN107903665 A CN 107903665A
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- CN
- China
- Prior art keywords
- zeolite powder
- silicone adhesive
- caprolactam
- preparation
- magnesium stearate
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
- C09C1/407—Aluminium oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- 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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of silicone adhesive modified zeolite powder, preparation method thereof, it is related to silicone adhesive technical field, comprises the following steps：（1）Prepare caprolactam magnesium stearate mixture；（2）Active zeolite powder；（3）Obtain pretreatment zeolite powder；（4）Obtain modified zeolite powder；The present invention is by being modified zeolite powder processing, the surface physicochemical property of zeolite powder can significantly be improved, improve its surface-active, it is applied to by the modified zeolite powder for obtaining the present invention in silicone adhesive, not only good dispersion, activity height, stability are good, also there is excellent high temperature resistant, antioxygenic property, not only can guarantee that colloid had good processing performance and mechanical property after applying it in silicone adhesive, but also significantly improve the high temperature resistant of colloid, ageing-resistant performance.
Description
Technical field
The invention belongs to silicone adhesive technical field, and in particular to a kind of silicone adhesive modified zeolite powder, preparation method thereof.
Background technology
Silicone sealant is mainly base by hydroxyl-terminated injecting two methyl siloxane as a kind of novel high polymer sealing material
Material, is aided with crosslinking agent, coupling agent, catalyst and filler and is formulated.Silicone adhesive has excellent weather resistance, and good is hydrophobic
Performance, excellent bio-compatible performance, is widely used and is led in building, electronic apparatus, aviation, automobile and medical and health etc.
Domain.Silicone sealant outdoor environment after by photo-thermal it is oxidizable degraded and harden cracking, it is this under higher temperature conditions
Degradation with aging is even more serious, it is impossible to meets the requirement of higher.
The content of the invention
The purpose of the present invention is for it is existing the problem of, there is provided a kind of silicone adhesive modified zeolite powder, preparation method thereof.
The present invention is achieved by the following technical solutions：
A kind of silicone adhesive modified zeolite powder, preparation method thereof, comprises the following steps：
(1) caprolactam is heated to molten condition, 30min is stirred at 350-400 DEG C, it is equal then to add magnesium stearate stirring
It is even, obtain caprolactam-magnesium stearate mixture；
(2) activator of its quality 3-5% is added into zeolite powder, after stirring evenly, then calcining 30- is carried out at 500-600 DEG C
35min, is then gas-cooled to room temperature；
(3) by step（1）In obtained caprolactam-magnesium stearate mixture be added in formic acid and dissolved, then again plus
Enter zeolite powder, be heated to 80 DEG C, when stirring 2 is small, is then filtered, cleaned using deionized water, drying to constant weight, obtains
To pretreatment zeolite powder；
(4) step (3) is obtained pretreatment zeolite powder to be added in organo-silicon coupling agent solution, into organo-silicon coupling agent solution
Add the maleic anhydride of its quality 2.5%, be heated to 80 DEG C, with 500r/min rotating speeds stirring 2 it is small when, then filtered,
After drying to constant weight at 200-250 DEG C, continue to keep the temperature 30min, then cooled to room temperature, to obtain the final product.
Further, the melting temperature of caprolactam is 155 DEG C in step (1), mole of caprolactam and magnesium stearate
Than for 1: 0.35mol.
Further, zeolite powder granularity is 1250 mesh in step (2).
Further, the step（2）Middle air cooling is that zeolite powder is carried out using 20 DEG C of nitrogen to continue cooling.
Further, the step（2）In activator be hexamethylene diisocyanate.
Further, caprolactam-magnesium stearate mixture presses 150g with formic acid in the step (3)：1550mL ratios
Mixing.
Further, the mass ratio of zeolite powder and caprolactam-magnesium stearate mixture is 5: 1 in the step (3).
Further, step (4) the organo-silicon coupling agent mass fraction is 7.5%.
The present invention has the following advantages compared with prior art：The present invention is by being modified zeolite powder processing, Neng Gou great
The surface physicochemical property of the improvement zeolite powder of amplitude, improves its surface-active, should by the modified zeolite powder for obtaining the present invention
Use in silicone adhesive, not only good dispersion, activity height, stability are good, also with excellent high temperature resistant, antioxygenic property, by it
Not only it can guarantee that colloid had good processing performance and mechanical property after being applied in silicone adhesive, but also significantly improved the resistance to of colloid
High temperature, ageing-resistant performance.This method carries out surface modification using caprolactam-magnesium stearate mixture to zeolite powder, can improve
Resistance to elevated temperatures, chemical stability and the good antioxygenic property of modified zeolite powder.The method of the present invention technique is simple, operation letter
Just, production cost is low, energy consumption is low, has preferable economic benefit and social benefit.
Embodiment
Embodiment 1
A kind of silicone adhesive modified zeolite powder, preparation method thereof, comprises the following steps：
(1) caprolactam is heated to molten condition, 30min is stirred at 350 DEG C, then added magnesium stearate and stir evenly,
Obtain caprolactam-magnesium stearate mixture；
(2) activator of its quality 3% is added into zeolite powder, after stirring evenly, then calcining 30min is carried out at 500 DEG C, so
After be gas-cooled to room temperature；
(3) by step（1）In obtained caprolactam-magnesium stearate mixture be added in formic acid and dissolved, then again plus
Enter zeolite powder, be heated to 80 DEG C, when stirring 2 is small, is then filtered, cleaned using deionized water, drying to constant weight, obtains
To pretreatment zeolite powder；
(4) step (3) is obtained pretreatment zeolite powder to be added in organo-silicon coupling agent solution, into organo-silicon coupling agent solution
Add the maleic anhydride of its quality 2.5%, be heated to 80 DEG C, with 500r/min rotating speeds stirring 2 it is small when, then filtered,
After drying to constant weight at 200 DEG C, continue to keep the temperature 30min, then cooled to room temperature, to obtain the final product.
Further, the melting temperature of caprolactam is 155 DEG C in step (1), mole of caprolactam and magnesium stearate
Than for 1: 0.35mol.
Further, zeolite powder granularity is 1250 mesh in step (2).
Further, the step（2）Middle air cooling is that zeolite powder is carried out using 20 DEG C of nitrogen to continue cooling.
Further, the step（2）In activator be hexamethylene diisocyanate.
Further, caprolactam-magnesium stearate mixture presses 150g with formic acid in the step (3)：1550mL ratios
Mixing.
Further, the mass ratio of zeolite powder and caprolactam-magnesium stearate mixture is 5: 1 in the step (3).
Further, step (4) the organo-silicon coupling agent mass fraction is 7.5%.
Embodiment 2
A kind of silicone adhesive modified zeolite powder, preparation method thereof, comprises the following steps：
(1) caprolactam is heated to molten condition, 30min is stirred at 400 DEG C, then added magnesium stearate and stir evenly,
Obtain caprolactam-magnesium stearate mixture；
(2) activator of its quality 5% is added into zeolite powder, after stirring evenly, then calcining 35min is carried out at 600 DEG C, so
After be gas-cooled to room temperature；
(3) by step（1）In obtained caprolactam-magnesium stearate mixture be added in formic acid and dissolved, then again plus
Enter zeolite powder, be heated to 80 DEG C, when stirring 2 is small, is then filtered, cleaned using deionized water, drying to constant weight, obtains
To pretreatment zeolite powder；
(4) step (3) is obtained pretreatment zeolite powder to be added in organo-silicon coupling agent solution, into organo-silicon coupling agent solution
Add the maleic anhydride of its quality 2.5%, be heated to 80 DEG C, with 500r/min rotating speeds stirring 2 it is small when, then filtered,
After drying to constant weight at 250 DEG C, continue to keep the temperature 30min, then cooled to room temperature, to obtain the final product.
Further, the melting temperature of caprolactam is 155 DEG C in step (1), mole of caprolactam and magnesium stearate
Than for 1: 0.35mol.
Further, zeolite powder granularity is 1250 mesh in step (2).
Further, the step（2）Middle air cooling is that zeolite powder is carried out using 20 DEG C of nitrogen to continue cooling.
Further, the step（2）In activator be hexamethylene diisocyanate.
Further, caprolactam-magnesium stearate mixture presses 150g with formic acid in the step (3)：1550mL ratios
Mixing.
Further, the mass ratio of zeolite powder and caprolactam-magnesium stearate mixture is 5: 1 in the step (3).
Further, step (4) the organo-silicon coupling agent mass fraction is 7.5%.
Embodiment 3
A kind of silicone adhesive modified zeolite powder, preparation method thereof, comprises the following steps：
(1) caprolactam is heated to molten condition, 30min is stirred at 380 DEG C, then added magnesium stearate and stir evenly,
Obtain caprolactam-magnesium stearate mixture；
(2) activator of its quality 4% is added into zeolite powder, after stirring evenly, then calcining 32min is carried out at 550 DEG C, so
After be gas-cooled to room temperature；
(3) by step（1）In obtained caprolactam-magnesium stearate mixture be added in formic acid and dissolved, then again plus
Enter zeolite powder, be heated to 80 DEG C, when stirring 2 is small, is then filtered, cleaned using deionized water, drying to constant weight, obtains
To pretreatment zeolite powder；
(4) step (3) is obtained pretreatment zeolite powder to be added in organo-silicon coupling agent solution, into organo-silicon coupling agent solution
Add the maleic anhydride of its quality 2.5%, be heated to 80 DEG C, with 500r/min rotating speeds stirring 2 it is small when, then filtered,
After drying to constant weight at 220 DEG C, continue to keep the temperature 30min, then cooled to room temperature, to obtain the final product.
Further, the melting temperature of caprolactam is 155 DEG C in step (1), mole of caprolactam and magnesium stearate
Than for 1: 0.35mol.
Further, zeolite powder granularity is 1250 mesh in step (2).
Further, the step（2）Middle air cooling is that zeolite powder is carried out using 20 DEG C of nitrogen to continue cooling.
Further, the step（2）In activator be hexamethylene diisocyanate.
Further, caprolactam-magnesium stearate mixture presses 150g with formic acid in the step (3)：1550mL ratios
Mixing.
Further, the mass ratio of zeolite powder and caprolactam-magnesium stearate mixture is 5: 1 in the step (3).
Further, step (4) the organo-silicon coupling agent mass fraction is 7.5%.
Experiment
Modified zeolite powder, common zeolite powder prepared by the present invention（Comparative example 1）And ordinary calcium carbonate（Comparative example 2）Press respectively
3:50 mass ratios are added in the preparation of commercially available silicone adhesive of the same race, and manufactured silicone adhesive performance is contrasted：
Experiment：
Table 1
| Traditional performance（Tensile strength MPa） | After ultraviolet ageing processing（Tensile strength MPa） | |
| Embodiment 1 | 3.12 | 2.58 |
| Embodiment 2 | 3.15 | 2.61 |
| Embodiment 3 | 3.10 | 2.55 |
| Comparative example 1 | 2.68 | 1.82 |
| Comparative example 2 | 2.79 | 1.95 |
As can be seen from Table 1, the modified zeolite powder that prepared by the present invention can effectively improve silicone adhesive ageing-resistant performance, and addition is general
Silicone adhesive prepared by logical calcium carbonate has more preferable tensile strength compared to the silicone adhesive for adding common zeolite powder preparation.
Claims (8)
1. a kind of silicone adhesive modified zeolite powder, preparation method thereof, it is characterised in that comprise the following steps：
(1) caprolactam is heated to molten condition, 30min is stirred at 350-400 DEG C, it is equal then to add magnesium stearate stirring
It is even, obtain caprolactam-magnesium stearate mixture；
(2) activator of its quality 3-5% is added into zeolite powder, after stirring evenly, then calcining 30- is carried out at 500-600 DEG C
35min, is then gas-cooled to room temperature；
(3) by step（1）In obtained caprolactam-magnesium stearate mixture be added in formic acid and dissolved, then again plus
Enter zeolite powder, be heated to 80 DEG C, when stirring 2 is small, is then filtered, cleaned using deionized water, drying to constant weight, obtains
To pretreatment zeolite powder；
(4) step (3) is obtained pretreatment zeolite powder to be added in organo-silicon coupling agent solution, into organo-silicon coupling agent solution
Add the maleic anhydride of its quality 2.5%, be heated to 80 DEG C, with 500r/min rotating speeds stirring 2 it is small when, then filtered,
After drying to constant weight at 200-250 DEG C, continue to keep the temperature 30min, then cooled to room temperature, to obtain the final product.
2. a kind of silicone adhesive modified zeolite powder, preparation method thereof according to claim 1, it is characterised in that in step (1)
The melting temperature of caprolactam is 155 DEG C, and the molar ratio of caprolactam and magnesium stearate is 1: 0.35mol.
3. a kind of silicone adhesive modified zeolite powder, preparation method thereof according to claim 1, it is characterised in that in step (2)
Zeolite powder granularity is 1250 mesh.
A kind of 4. silicone adhesive modified zeolite powder, preparation method thereof according to claim 1, it is characterised in that the step
（2）Middle air cooling is that zeolite powder is carried out using 20 DEG C of nitrogen to continue cooling.
A kind of 5. silicone adhesive modified zeolite powder, preparation method thereof according to claim 1, it is characterised in that the step
（2）In activator be hexamethylene diisocyanate.
A kind of 6. silicone adhesive modified zeolite powder, preparation method thereof according to claim 1, it is characterised in that the step
(3) caprolactam-magnesium stearate mixture presses 150g with formic acid in：1550mL ratios mix.
A kind of 7. silicone adhesive modified zeolite powder, preparation method thereof described in a square claim 1, it is characterised in that the step
(3) mass ratio of zeolite powder and caprolactam-magnesium stearate mixture is 5: 1 in.
A kind of 8. silicone adhesive modified zeolite powder, preparation method thereof according to claim 1, it is characterised in that the step
(4) organo-silicon coupling agent mass fraction is 7.5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711217985.3A CN107903665A (en) | 2017-11-28 | 2017-11-28 | A kind of silicone adhesive modified zeolite powder, preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711217985.3A CN107903665A (en) | 2017-11-28 | 2017-11-28 | A kind of silicone adhesive modified zeolite powder, preparation method thereof |
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| Publication Number | Publication Date |
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| CN107903665A true CN107903665A (en) | 2018-04-13 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103788781A (en) * | 2014-02-20 | 2014-05-14 | 铜陵祥云消防科技有限责任公司 | Modified nano zeolite powder added fireproof coating material |
| CN105368378A (en) * | 2015-12-18 | 2016-03-02 | 广州市白云化工实业有限公司 | Silicone sealant with finishing capacity and preparation method of silicone sealant |
| CN106750798A (en) * | 2016-12-20 | 2017-05-31 | 安徽新立电缆材料有限公司 | A kind of acid and alkali-resistance waterproof polyethylene cable material |
| CN107286641A (en) * | 2017-06-21 | 2017-10-24 | 东莞市联洲知识产权运营管理有限公司 | A kind of polyether sulfone based on nano-attapulgite/nylon composite heat resistance material and preparation method thereof |
-
2017
- 2017-11-28 CN CN201711217985.3A patent/CN107903665A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103788781A (en) * | 2014-02-20 | 2014-05-14 | 铜陵祥云消防科技有限责任公司 | Modified nano zeolite powder added fireproof coating material |
| CN105368378A (en) * | 2015-12-18 | 2016-03-02 | 广州市白云化工实业有限公司 | Silicone sealant with finishing capacity and preparation method of silicone sealant |
| CN106750798A (en) * | 2016-12-20 | 2017-05-31 | 安徽新立电缆材料有限公司 | A kind of acid and alkali-resistance waterproof polyethylene cable material |
| CN107286641A (en) * | 2017-06-21 | 2017-10-24 | 东莞市联洲知识产权运营管理有限公司 | A kind of polyether sulfone based on nano-attapulgite/nylon composite heat resistance material and preparation method thereof |
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Application publication date: 20180413 |
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