CN103468193A - Low-halogen low-smell epoxy resin pouring sealant and preparation process thereof - Google Patents
Low-halogen low-smell epoxy resin pouring sealant and preparation process thereof Download PDFInfo
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- CN103468193A CN103468193A CN2013104264771A CN201310426477A CN103468193A CN 103468193 A CN103468193 A CN 103468193A CN 2013104264771 A CN2013104264771 A CN 2013104264771A CN 201310426477 A CN201310426477 A CN 201310426477A CN 103468193 A CN103468193 A CN 103468193A
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Abstract
The invention provides a low-halogen low-smell epoxy resin pouring sealant and a preparation process thereof. The pouring sealant comprises a resin part and a curing agent part, wherein the resin part comprises the following components in parts by weight: 30-60 parts of bisphenol A-type epoxy resin, 5-15 parts of low-halogen diluting agent, 30-50 parts of filler, and 0-3 parts of auxiliaries; the curing agent part comprises the following components in parts by weight: 70-90 parts of alicyclic amine and 10-30 parts of low-halogen diluting agent; the ratio of the resin part to the curing agent part is 100: (20-40). The preparation process comprises the following steps of: (1) uniformly mixing the raw materials of the resin part, vacuumizing, and heating to a temperature of 40-60 DEG C; (2) heating the alicyclic amine of the curing agent part to a temperature of 60-70 DEG C, and dripping the low-halogen diluting agent while stirring; (3) uniformly mixing the product obtained in the step (1) and the product obtained in the step (2), wherein the diluting agent is added according to the adding amount that the content of halogen of the product cannot exceed the environment-friendly standard, namely 900PPM. The curing agent and the resin react with the low-halogen diluting agent before being mixed and used, so that the smell can be reduced, and the content of halogen cannot exceed the standard.
Description
Technical field
The present invention relates to a kind of joint sealant and preparation technology thereof, specifically, relate to epoxy resin embedding adhesive and the preparation technology thereof of the low smell of a kind of low halogen.
Background technology
Joint sealant of the prior art, generally adopt the thinner that content of halogen is tens thousand of PPM, in the situation that addition is 10% left and right, content of halogen far surpasses the 900PPM that European countries' high-environmental requires, and adopt while hanging down the halogen thinner, the viscosity of product, glass transition temperature Tg, the performance of water-intake rate is difficult to again work in coordination with.In addition, the amine curing agent that common joint sealant adopts has dense smell, is unfavorable for the manual operation use.
Summary of the invention
The object of the invention is to, when selecting low halogen thinner, by choosing suitable raw material and proportioning thereof, obtain the product of suitable viscosity, glass transition temperature Tg and water-intake rate.Another object of the present invention is to reduce the smell of joint sealant, the manual operation during for use offers convenience.
The present invention is achieved by the following technical solutions:
The prepared low halogen of the present invention hangs down the epoxy resin embedding adhesive of smell, comprises the component of following parts by weight:
(1) resin part, comprise 30～60 parts of bisphenol A type epoxy resins; 5～15 parts of low halogen thinners; 30～50 parts of fillers; 0～3 part of auxiliary agent; (2) curing agent part, comprise 70～90 parts of aliphatic cyclic amines; 10～30 parts of low halogen thinners; Described resin part is 100:20～40 with the ratio of curing agent part.
Further, described auxiliary agent comprises coupling agent, flow agent and defoamer.
Further, described low halogen thinner refers to that content of halogen is no more than the thinner of 3000PPM.
The preparation technology of the epoxy resin embedding adhesive of the low smell of low halogen of the present invention, comprise the steps:
(1) the described raw material of resin part is mixed in described ratio, vacuumize, and be warming up to 40～60 ℃, stir evenly; (2) aliphatic cyclic amine of curing agent part is heated to 60～70 ℃, splashes into low halogen thinner when stirring; (3) step (1) and the product of the middle gained of step (2) are mixed;
Above-mentioned resin portion is divided and is comprised, 30～60 parts of bisphenol A type epoxy resins; 5～15 parts of low halogen thinners; 30～50 parts of fillers; 0～3 part of auxiliary agent; Above-mentioned curing agent part comprises, 70～90 parts of aliphatic cyclic amines; 10～30 parts of low halogen thinners; Described resin part is 100:20～40 with the ratio of curing agent part.
Further, in step (1), vacuum degree control is at 700～760mm mercury column, and temperature is controlled at 45～50 ℃.
Temperature while mixing in step (3) further, is 25～35 ℃.
Further, described auxiliary agent comprises coupling agent, flow agent and defoamer.
Further, described low halogen thinner refers to that content of halogen is no more than the thinner of 3000PPM.
Further right, the prepared products solidifying condition of step (3) is that ambient cure is carried out hot setting at least 2 hours more than 24 hours or more than 70 ℃.
The low halogen thinner of selecting mainly comprises the thinner of low-halogen-contents such as being similar to alkyl glycidyl ether, neodecanoic acid Racemic glycidol fat, toluene glycidyl ether; Described aliphatic cyclic amine is the aliphatic cyclic amines commonly used such as peppermint diamines, N-aminoethyl piperazine, isophorone diamine, methyl ring pentamethylene diamine; Filler adopts the chemical fillers commonly used such as barium sulfate, calcium carbonate to get final product.
Beneficial effect of the present invention is: now low halogen thinner is under above-mentioned addition, and the product content of halogen made can not surpass the environmental requirement standard of existing 900PPM.Simultaneously, the present invention is directed to the problem that there is larger smell in amine curing agent, solidifying agent is being reacted with it by low halogen thinner with before the mixed with resin use, thereby reduction smell and halogen can not exceed standard.About the performance data and the effect that make product, can in conjunction with test data, be discussed in the embodiment part.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further:
Embodiment 1
(1) the described raw material of resin part is mixed in described ratio, vacuumize, and be warming up to 45 ℃, stir evenly; (2) aliphatic cyclic amine of curing agent part is heated to 70 ℃, splashes into low halogen thinner when stirring; (3) step (1) and the product of the middle gained of step (2) are mixed; Above-mentioned resin portion is divided and is comprised, 50 parts of bisphenol A type epoxy resins; 12 parts of low halogen thinners; 37 parts of fillers; 2 parts of auxiliary agents; Above-mentioned curing agent part comprises, 75 parts of aliphatic cyclic amines; 20 parts of low halogen thinners; Described resin part is 100:30 with the ratio of curing agent part.
In step (1), vacuum degree control is at the 710mm mercury column, and temperature is controlled at 50 ℃.Temperature while mixing in step (3) is 25 ℃.Described auxiliary agent comprises coupling agent, flow agent and defoamer.Thinner is all selected the alkyl glycidyl ether of low-halogen-content; Filler adopts calcium carbonate; The aliphatic cyclic amine part can be for methyl ring pentamethylene diamine as solidifying agent.
While being cured, the prepared products solidifying condition of step (3) is that ambient cure is carried out hot setting at least 2 hours more than 24 hours or more than 70 ℃.
Embodiment 2
(1) the described raw material of resin part is mixed in described ratio, vacuumize, and be warming up to 45 ℃, stir evenly; (2) aliphatic cyclic amine of curing agent part is heated to 68 ℃, splashes into low halogen thinner when stirring; (3) step (1) and the product of the middle gained of step (2) are mixed; Above-mentioned resin portion is divided and is comprised, 35 parts of bisphenol A type epoxy resins; 15 parts of low halogen thinners; 48 parts of fillers; 1 part of auxiliary agent; Above-mentioned curing agent part comprises, 87 parts of aliphatic cyclic amines; 15 parts of low halogen thinners; Described resin part is 100:35 with the ratio of curing agent part.
In step (1), vacuum degree control is at the 750mm mercury column, and temperature is controlled at 46 ℃.Temperature while mixing in step (3) is 32 ℃.Described auxiliary agent comprises coupling agent, flow agent and defoamer.Thinner is all selected the toluene glycidyl ether of low-halogen-content; Filler adopts calcium carbonate; The aliphatic cyclic amine part can be for isophorone diamine as solidifying agent.
While being cured, the prepared products solidifying condition of step (3) is that ambient cure is carried out hot setting at least 2 hours more than 24 hours or more than 70 ℃.
We carry out contrast test to the usual production on following examples and market, and result is as follows:
In form, data can be found out, after commercially available prod has adopted low halogen thinner, its water-intake rate improves, and is unfavorable for protection against the tide, and weather resistance significantly reduces, and products obtained therefrom of the present invention has met the requirement of low halogen and moistureproof weather resistance simultaneously.
The foregoing is only the preferred embodiment of this patent, can not be interpreted as limitation of the present invention, on basis of the present invention, the equivalent technical solutions that those skilled in the art can association draw according to above disclosed content still falls into the protection domain of this patent.
Claims (9)
1. the epoxy resin embedding adhesive of the low smell of a low halogen comprises the component of following parts by weight:
(1) resin part, comprise 30～60 parts of bisphenol A type epoxy resins; 5～15 parts of low halogen thinners; 30～50 parts of fillers; 0～3 part of auxiliary agent; (2) curing agent part, comprise 70～90 parts of aliphatic cyclic amines; 10～30 parts of low halogen thinners; Described resin part is 100:20～40 with the ratio of curing agent part.
2. low halogen according to claim 1 hangs down the epoxy resin embedding adhesive of smell, and it is characterized in that: described auxiliary agent comprises coupling agent, flow agent and defoamer.
3. low halogen according to claim 1 and 2 hangs down the epoxy resin embedding adhesive of smell, and it is characterized in that: described low halogen thinner refers to that content of halogen is no more than the thinner of 3000PPM.
4. the preparation technology of the epoxy resin embedding adhesive of the low smell of low halogen, comprise the steps:
(1) the described raw material of resin part is mixed in described ratio, vacuumize, and be warming up to 40～60 ℃, stir evenly; (2) aliphatic cyclic amine of curing agent part is heated to 60～70 ℃, splashes into low halogen thinner when stirring; (3) step (1) and the product of the middle gained of step (2) are mixed;
Above-mentioned resin portion is divided and is comprised, 30～60 parts of bisphenol A type epoxy resins; 5～15 parts of low halogen thinners; 30～50 parts of fillers; 0～3 part of auxiliary agent; Above-mentioned curing agent part comprises, 70～90 parts of aliphatic cyclic amines; 10～30 parts of low halogen thinners; Described resin part is 100:20～40 with the ratio of curing agent part.
5. hang down the preparation technology of the epoxy resin embedding adhesive of smell according to low halogen claimed in claim 4, it is characterized in that: in step (1), vacuum degree control is at 700～760mm mercury column, and temperature is controlled at 45～50 ℃.
6. hang down the preparation technology of the epoxy resin embedding adhesive of smell according to low halogen claimed in claim 4, it is characterized in that: the temperature while mixing in step (3) is 25～35 ℃.
7. hang down the preparation technology of the epoxy resin embedding adhesive of smell according to low halogen claimed in claim 4, it is characterized in that: described auxiliary agent comprises coupling agent, flow agent and defoamer.
8. hang down the preparation technology of the epoxy resin embedding adhesive of smell according to low halogen claimed in claim 4, it is characterized in that: described low halogen thinner refers to that content of halogen is no more than the thinner of 3000PPM.
9. hang down the preparation technology of the epoxy resin embedding adhesive of smell according to the described low halogen of any one in claim 4-8, it is characterized in that: the prepared products solidifying condition of step (3) is that ambient cure is carried out hot setting at least 2 hours more than 24 hours or more than 70 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310426477.1A CN103468193B (en) | 2013-09-17 | 2013-09-17 | Epoxy resin embedding adhesive and the preparation technology thereof of the low smell of low halogen |
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| CN201310426477.1A CN103468193B (en) | 2013-09-17 | 2013-09-17 | Epoxy resin embedding adhesive and the preparation technology thereof of the low smell of low halogen |
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| CN103468193B CN103468193B (en) | 2016-05-18 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115368857A (en) * | 2022-08-23 | 2022-11-22 | 书香门地集团股份有限公司 | Anti-cracking low-halogen low-transparency epoxy resin sealant |
Citations (4)
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|---|---|---|---|---|
| US20100155123A1 (en) * | 2008-12-22 | 2010-06-24 | Iteq Corporation | Halogen-free prepreg and resin for preparing the same |
| CN102516914A (en) * | 2011-11-21 | 2012-06-27 | 烟台德邦电子材料有限公司 | Halogen-free flame-retardant epoxy resin electronic pouring sealant |
| JP2012211244A (en) * | 2011-03-31 | 2012-11-01 | Aica Kogyo Co Ltd | Epoxy resin adhesive composition |
| CN102850988A (en) * | 2012-09-26 | 2013-01-02 | 中南大学 | Epoxy resin pouring sealant and usage method |
-
2013
- 2013-09-17 CN CN201310426477.1A patent/CN103468193B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100155123A1 (en) * | 2008-12-22 | 2010-06-24 | Iteq Corporation | Halogen-free prepreg and resin for preparing the same |
| JP2012211244A (en) * | 2011-03-31 | 2012-11-01 | Aica Kogyo Co Ltd | Epoxy resin adhesive composition |
| CN102516914A (en) * | 2011-11-21 | 2012-06-27 | 烟台德邦电子材料有限公司 | Halogen-free flame-retardant epoxy resin electronic pouring sealant |
| CN102850988A (en) * | 2012-09-26 | 2013-01-02 | 中南大学 | Epoxy resin pouring sealant and usage method |
Non-Patent Citations (1)
| Title |
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| 贺曼罗: "《环氧树脂胶粘剂》", 30 April 2004, 中国石化出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115368857A (en) * | 2022-08-23 | 2022-11-22 | 书香门地集团股份有限公司 | Anti-cracking low-halogen low-transparency epoxy resin sealant |
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