CN103805123B - Adhesive containing modified silica powder - Google Patents

Adhesive containing modified silica powder Download PDF

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Publication number
CN103805123B
CN103805123B CN201410058066.6A CN201410058066A CN103805123B CN 103805123 B CN103805123 B CN 103805123B CN 201410058066 A CN201410058066 A CN 201410058066A CN 103805123 B CN103805123 B CN 103805123B
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parts
micro mist
powder
modified silicon
containing modified
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CN201410058066.6A
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CN103805123A (en
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何益庆
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Shenzhen Meizhi Electric Industry Co., Ltd.
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Tongling Xiangyun Fire Fighting Technology Co Ltd
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Abstract

The invention discloses an adhesive containing modified silica powder. The adhesive is prepared by the following raw materials in parts by weight: 50-100 parts of phenolic group propane epoxy resin, 50-80 parts of ethyl acetate, 40-60 parts of toluene diisocynate, 3-5 parts of poly tetrahydrofuran ether glycol, 5-8 parts of cellulose ether, 5-10 parts of nitrile rubber, 3-5 parts of epoxidized soybean oil, 1-3 parts of boron powder, 10-15 parts of modified silica powder, 5-10 parts of fumed silica, 2-4 parts of nanometer titanium dioxide, 1-3 parts of ferrocene, 2-3 parts of magnesium oxide, 3-5 parts of silica fume, 0.5-0.8 part of dibutyltin dilaurate, 0.3-0.5 part of phosphoric acid, 2-4 parts of sodium silicate, 2-4 parts of antiager MB, 2-4 parts of accelerant BZ, 1-3 parts of silane coupling agent, 2-4 parts of scorch retarder, 2-4 parts of flexibilizer DY-040, and 10-15 parts of modified ash tree. The adhesive has characteristics of high compression resistance, high bonding strength, and good heat and humidity resistance, and can be used for bonding in occasions with requirements on high strength and heat and humidity resistance.

Description

A kind of sizing agent containing modified silicon micro mist
Technical field
The present invention relates to sizing agent technical field, particularly relate to a kind of sizing agent containing modified silicon micro mist.
Background technology
Sizing agent is a kind of material that similar or inhomogeneous material tight can be combined.Along with development that is scientific and technical and national economy, tackiness agent has been widely used in every profession and trade and the high-tech areas such as wood working, construction work, textile printing and dyeing, shoemaking, leather, electronics, automobile, machinery, aerospace, biologic medical.
Current sizing agent ubiquity the shortcoming that curing speed is slow, poor heat resistance, winter hardiness are not good, package stability is poor.The shortcomings such as low in order to overcome traditional sizing agent intensity, humidity resistance is not good, package stability difference, by improving formula, thus produce a kind of Novel adhesive.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of high resistance to compression, good impact resistance, humidity resistance good, the sizing agent containing modified silicon micro mist that period of storage is long.
The present invention adopts following technical scheme to achieve these goals:
A kind of sizing agent containing modified silicon micro mist, be made up of the raw material of following weight part: phenolic group propane epoxy resin 50-100 part, ethyl acetate 50-80 part, tolylene diisocyanate 40-60 part, PTMG 3-5 part, ether of cellulose 5-8 part, paracril 5-10 part, epoxy soybean oil 3-5 part, boron powder 1-3 part, modified silicon micro mist 10-15 part, gas-phase silica 5-10 part, nano titanium oxide 2-4 part, ferrocene 1-3 part, magnesium oxide 2-3 part, silicon ash 3-5 part, dibutyl tin laurate 0.5-0.8 part, phosphoric acid 0.3-0.5 part, water glass 2-4 part, antioxidant MB 2-4 part, accelerant B Z 2-4 part, silane coupling agent 1-3 part, scorch retarder 2-4 part, toughner DY-040 2-4 part, modification tree ash 10-15 part.
Described modified silicon micro mist is prepared by following steps: first carry out surface cleaning with argon gas to silicon powder, then the silicon powder after cleaning is put into reaction flask, add and be equivalent to the pyrroles of silicon powder weight 2-4%, 1 of 3-5%, the vinylformic acid of 3-diaminopropanes, 2-4%, the silane coupling agent of 2-4%, stir, under vacuum, use the RF Plasma Discharge that rf frequency is 10-15MHz, discharge power is 100-120W, discharge time is 60-80s, obtains the silicon powder of modification.
Described modification tree ash is obtained by following steps: first use 10-15% salt acid soak tree ash 3-5h, then clean with deionized water wash, 3-5h is soaked again with 10-13% sodium hydroxide solution, extremely neutral with deionized water wash again, dry, add be equivalent to tree ash weight 2-4% wooden sodium sulfonate, the peregal of 1-3%, the tributyl citrate of 2-4%, the Sumstar 190 of 2-4%, high speed 1300-1500 rev/min stir 1-3h, pulverize grind to form ultrafine powder.
The preparation method of the described sizing agent containing modified silicon micro mist, comprises following preparation process:
(1) by above-mentioned weight ratio, phenolic group propane epoxy resin, ethyl acetate, tolylene diisocyanate, PTMG, ether of cellulose, paracril, ferrocene, dibutyl tin laurate, phosphoric acid, water glass are added reactor and are heated to 100-120 DEG C, high-speed stirring 2-3h;
(2) other material is mixed with reactant in step (1), stir 30-50min, be cooled to normal temperature, obtain finished product, pack.
Compared with the prior art, beneficial effect of the present invention is as follows:
The present invention is by adding modified silicon micro mist, and modified silicon micro mist not only can improve itself and the combination of polymkeric substance, also improves toughness of products and shock resistance, and the enhancing of coated power, has good activity degree.Joined in sizing agent, change formula, the sizing agent obtained is had features such as intensity is high, wet-heat resisting, may be used for the bonding of the occasions such as desired strength is high, wet-heat resisting.Meanwhile, modification is carried out to tree ash, improve the dispersing uniformity of sizing agent component, obviously can improve bonding strength and the water tolerance of sizing agent.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1:
A kind of sizing agent containing modified silicon micro mist, be made up of the raw material of following weight part: phenolic group propane epoxy resin 50 parts, ethyl acetate 70 parts, tolylene diisocyanate 40 parts, PTMG 3 parts, ether of cellulose 6 parts, paracril 7 parts, epoxy soybean oil 3 parts, 1 part, boron powder, modified silicon micro mist 10 parts, gas-phase silica 5 parts, nano titanium oxide 2 parts, ferrocene 1 part, 2 parts, magnesium oxide, silicon ash 3 parts, dibutyl tin laurate 0.5 part, phosphoric acid 0.3 part, water glass 2 parts, antioxidant MB 2 parts, accelerant B Z 2 parts, silane coupling agent 1 part, scorch retarder 2 parts, toughner DY-040 2 parts, modification tree ash 10 parts.
Modified silicon micro mist is prepared by following steps: first carry out surface cleaning with argon gas to silicon powder, then the silicon powder after cleaning is put into reaction flask, add and be equivalent to the pyrroles of silicon powder weight 2%, 3% 1,3-diaminopropanes, the vinylformic acid of 2%, the silane coupling agent of 2%, stir, under vacuum, use the RF Plasma Discharge that rf frequency is 10MHz, discharge power is 100W, discharge time is 60s, obtains the silicon powder of modification.
Modification tree ash is obtained by following steps: first use 10% salt acid soak tree ash 3h, then clean with deionized water wash, 3h is soaked again with 10% sodium hydroxide solution, extremely neutral with deionized water wash again, dry, add be equivalent to tree ash weight 2% wooden sodium sulfonate, 1% peregal, the tributyl citrate of 2%, the Sumstar 190 of 2%, at a high speed 1300 revs/min are stirred 1h, pulverize and grind to form ultrafine powder.
The preparation method of the sizing agent containing modified silicon micro mist, comprises following preparation process:
(1) by above-mentioned weight ratio, phenolic group propane epoxy resin, ethyl acetate, tolylene diisocyanate, PTMG, ether of cellulose, paracril, ferrocene, dibutyl tin laurate, phosphoric acid, water glass are added reactor and be heated to 100 DEG C, high-speed stirring 2h;
(2) other material is mixed with reactant in step (1), stir 40min, be cooled to normal temperature, obtain finished product, pack.
Embodiment 2:
A kind of sizing agent containing modified silicon micro mist, be made up of the raw material of following weight part: phenolic group propane epoxy resin 100 parts, ethyl acetate 80 parts, tolylene diisocyanate 60 parts, PTMG 5 parts, ether of cellulose 8 parts, paracril 10 parts, epoxy soybean oil 5 parts, 3 parts, boron powder, modified silicon micro mist 15 parts, gas-phase silica 10 parts, nano titanium oxide 4 parts, ferrocene 3 parts, 3 parts, magnesium oxide, silicon ash 5 parts, dibutyl tin laurate 0.8 part, phosphoric acid 0.5 part, water glass 4 parts, antioxidant MB 4 parts, accelerant B Z 4 parts, silane coupling agent 3 parts, scorch retarder 4 parts, toughner DY-040 4 parts, modification tree ash 15 parts.
Modified silicon micro mist is prepared by following steps: first carry out surface cleaning with argon gas to silicon powder, then the silicon powder after cleaning is put into reaction flask, add and be equivalent to the pyrroles of silicon powder weight 4%, 5% 1,3-diaminopropanes, the vinylformic acid of 4%, the silane coupling agent of 4%, stir, under vacuum, use the RF Plasma Discharge that rf frequency is 15MHz, discharge power is 120W, discharge time is 80s, obtains the silicon powder of modification.
Modification tree ash is obtained by following steps: first use 15% salt acid soak tree ash 5h, then clean with deionized water wash, 5h is soaked again with 13% sodium hydroxide solution, extremely neutral with deionized water wash again, dry, add be equivalent to tree ash weight 4% wooden sodium sulfonate, 3% peregal, the tributyl citrate of 4%, the Sumstar 190 of 4%, at a high speed 1500 revs/min are stirred 3h, pulverize and grind to form ultrafine powder.
The preparation method of the sizing agent containing modified silicon micro mist, comprises following preparation process:
(1) by above-mentioned weight ratio, phenolic group propane epoxy resin, ethyl acetate, tolylene diisocyanate, PTMG, ether of cellulose, paracril, ferrocene, dibutyl tin laurate, phosphoric acid, water glass are added reactor and be heated to 120 DEG C, high-speed stirring 3h;
(2) other material is mixed with reactant in step (1), stir 50min, be cooled to normal temperature, obtain finished product, pack.
Embodiment 3:
A kind of sizing agent containing modified silicon micro mist, be made up of the raw material of following weight part: phenolic group propane epoxy resin 80 parts, ethyl acetate 70 parts, tolylene diisocyanate 50 parts, PTMG 4 parts, ether of cellulose 7 parts, paracril 9 parts, epoxy soybean oil 4 parts, 2 parts, boron powder, modified silicon micro mist 13 parts, gas-phase silica 8 parts, nano titanium oxide 3 parts, ferrocene 2 parts, 3 parts, magnesium oxide, silicon ash 4 parts, dibutyl tin laurate 0.6 part, phosphoric acid 0.4 part, water glass 3 parts, antioxidant MB 3 parts, accelerant B Z 3 parts, silane coupling agent 2 parts, scorch retarder 3 parts, toughner DY-040 3 parts, modification tree ash 11 parts.
Modified silicon micro mist is prepared by following steps: first carry out surface cleaning with argon gas to silicon powder, then the silicon powder after cleaning is put into reaction flask, add and be equivalent to the pyrroles of silicon powder weight 3%, 4% 1,3-diaminopropanes, the vinylformic acid of 3%, the silane coupling agent of 3%, stir, under vacuum, use the RF Plasma Discharge that rf frequency is 15MHz, discharge power is 120W, discharge time is 70s, obtains the silicon powder of modification.
Modification tree ash is obtained by following steps: first use 15% salt acid soak tree ash 4h, then clean with deionized water wash, 4h is soaked again with 10% sodium hydroxide solution, extremely neutral with deionized water wash again, dry, add be equivalent to tree ash weight 3% wooden sodium sulfonate, 2% peregal, the tributyl citrate of 3%, the Sumstar 190 of 3%, at a high speed 1500 revs/min are stirred 2h, pulverize and grind to form ultrafine powder.
The preparation method of the described sizing agent containing modified silicon micro mist, comprises following preparation process:
(1) by above-mentioned weight ratio, phenolic group propane epoxy resin, ethyl acetate, tolylene diisocyanate, PTMG, ether of cellulose, paracril, ferrocene, dibutyl tin laurate, phosphoric acid, water glass are added reactor and be heated to 100 DEG C, high-speed stirring 3h;
(2) other material is mixed with reactant in step (1), stir 50min, be cooled to normal temperature, obtain finished product, pack.
Sizing agent prepared by the present embodiment 1 and traditional sizing agent performance test are as following table 1:
Table 1:

Claims (2)

1. the sizing agent containing modified silicon micro mist, it is characterized in that: be made up of the raw material of following weight part: phenolic group propane epoxy resin 50-100 part, ethyl acetate 50-80 part, tolylene diisocyanate 40-60 part, PTMG 3-5 part, ether of cellulose 5-8 part, paracril 5-10 part, epoxy soybean oil 3-5 part, boron powder 1-3 part, modified silicon micro mist 10-15 part, gas-phase silica 5-10 part, nano titanium oxide 2-4 part, ferrocene 1-3 part, magnesium oxide 2-3 part, silicon ash 3-5 part, dibutyl tin laurate 0.5-0.8 part, phosphoric acid 0.3-0.5 part, water glass 2-4 part, antioxidant MB 2-4 part, accelerant B Z 2-4 part, silane coupling agent 1-3 part, scorch retarder 2-4 part, toughner DY-040 2-4 part, modification tree ash 10-15 part,
Described modified silicon micro mist is prepared by following steps: first carry out surface cleaning with argon gas to silicon powder, then the silicon powder after cleaning is put into reaction flask, add and be equivalent to the pyrroles of silicon powder weight 2-4%, 1 of 3-5%, the vinylformic acid of 3-diaminopropanes, 2-4%, the silane coupling agent of 2-4%, stir, under vacuum, use the RF Plasma Discharge that rf frequency is 10-15MHz, discharge power is 100-120W, discharge time is 60-80s, obtains the silicon powder of modification;
Described modification tree ash is obtained by following steps: first use 10-15% salt acid soak tree ash 3-5h, then clean with deionized water wash, 3-5h is soaked again with 10-13% sodium hydroxide solution, extremely neutral with deionized water wash again, dry, add be equivalent to tree ash weight 2-4% wooden sodium sulfonate, the peregal of 1-3%, the tributyl citrate of 2-4%, the Sumstar 190 of 2-4%, high speed 1300-1500 rev/min stir 1-3h, pulverize grind to form ultrafine powder;
The preparation method of the described sizing agent containing modified silicon micro mist, comprises following preparation process:
(1) by above-mentioned weight ratio, phenolic group propane epoxy resin, ethyl acetate, tolylene diisocyanate, PTMG, ether of cellulose, paracril, ferrocene, dibutyl tin laurate, phosphoric acid, water glass are added reactor and are heated to 100-120 DEG C, high-speed stirring 2-3h;
(2) other material is mixed with reactant in step (1), stir 30-50min, be cooled to normal temperature, obtain finished product, pack.
2. a preparation method for the sizing agent containing modified silicon micro mist as claimed in claim 1, is characterized in that: comprise following preparation process:
(1) by above-mentioned weight ratio, phenolic group propane epoxy resin, ethyl acetate, tolylene diisocyanate, PTMG, ether of cellulose, paracril, ferrocene, dibutyl tin laurate, phosphoric acid, water glass are added reactor and are heated to 100-120 DEG C, high-speed stirring 2-3h;
(2) other material is mixed with reactant in step (1), stir 30-50min, be cooled to normal temperature, obtain finished product, pack.
CN201410058066.6A 2014-02-20 2014-02-20 Adhesive containing modified silica powder Expired - Fee Related CN103805123B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100576907B1 (en) * 2002-12-24 2006-05-03 (주) 존인피니티 Primer composition for hot fix of textile and crystal rhine stone and aluminum stud having primer layer formed thereby
CN102965050A (en) * 2012-11-02 2013-03-13 铜陵祥云消防科技有限责任公司 Nano-kieselguhr modified adhesive for packaging
CN102965036A (en) * 2012-11-02 2013-03-13 铜陵祥云消防科技有限责任公司 Nano-wollastonite modified adhesive for packaging
CN103059750A (en) * 2012-12-14 2013-04-24 铜陵市铜运机械有限公司 Epoxy resin and nitrile rubber adhesive and preparing method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100576907B1 (en) * 2002-12-24 2006-05-03 (주) 존인피니티 Primer composition for hot fix of textile and crystal rhine stone and aluminum stud having primer layer formed thereby
CN102965050A (en) * 2012-11-02 2013-03-13 铜陵祥云消防科技有限责任公司 Nano-kieselguhr modified adhesive for packaging
CN102965036A (en) * 2012-11-02 2013-03-13 铜陵祥云消防科技有限责任公司 Nano-wollastonite modified adhesive for packaging
CN103059750A (en) * 2012-12-14 2013-04-24 铜陵市铜运机械有限公司 Epoxy resin and nitrile rubber adhesive and preparing method thereof

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Effective date of registration: 20161221

Address after: 542899 Hezhou the Guangxi Zhuang Autonomous Region Electronic Science and technology park is run on the road No. 1

Patentee after: Guangxi Huizhi Productivity Promotion Center Co. Ltd.

Address before: 244100 Tongling Jinqiao Industrial Park, Tongling, Anhui

Patentee before: Tongling Xiangyun Fire-fighting Technology Co., Ltd.

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Effective date of registration: 20190418

Address after: 518055 Dong 401-404, No. 5, Honghualing Industrial Zone, Taoyuan Street, Nanshan District, Shenzhen City, Guangdong Province

Patentee after: Shenzhen Meizhi Electric Industry Co., Ltd.

Address before: 542899 No. 1 Zhengrun Avenue, Hezhou Electronic Science and Technology Park, Guangxi Zhuang Autonomous Region

Patentee before: Guangxi Huizhi Productivity Promotion Center Co. Ltd.

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Granted publication date: 20150701

Termination date: 20200220