CN103374115A - Preparation method of modified epoxy resin - Google Patents

Preparation method of modified epoxy resin Download PDF

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Publication number
CN103374115A
CN103374115A CN2013102733943A CN201310273394A CN103374115A CN 103374115 A CN103374115 A CN 103374115A CN 2013102733943 A CN2013102733943 A CN 2013102733943A CN 201310273394 A CN201310273394 A CN 201310273394A CN 103374115 A CN103374115 A CN 103374115A
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CN
China
Prior art keywords
epoxy
preparation
polyethers
modified
montmorillonite
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Pending
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CN2013102733943A
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Chinese (zh)
Inventor
刘荣春
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NANJING RONGDA RESIN Co Ltd
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NANJING RONGDA RESIN Co Ltd
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Priority to CN2013102733943A priority Critical patent/CN103374115A/en
Publication of CN103374115A publication Critical patent/CN103374115A/en
Pending legal-status Critical Current

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  • Polyurethanes Or Polyureas (AREA)
  • Epoxy Resins (AREA)

Abstract

The invention discloses a preparation method of a modified epoxy resin, which comprises the following steps: organizing montmorillonite; preparation of polyether intercalated montmorillonite from organized montmorillonite: adding the organized 30% organic montmorillonite into polyether N-210, dispersing by stirring, and grinding to obtain polyether intercalated montmorillonite powder; synthesizing a polyurethane prepolymer; stirring TDI (toluene diisocyanate) and the polyether intercalated montmorillonite powder to react to obtain a nano modified polyurethane prepolymer; mixing the nano modified polyurethane prepolymer with an epoxy resin, and stirring to react to obtain an epoxy modified body, wherein the mass ratio of the nano modified polyurethane prepolymer to the epoxy resin is 1:(1.8-2.5); and finally, curing the epoxy modified body and a curing agent polyamide in a mass ratio of 40:(1.8-2.5) to form. The epoxy resin prepared by the method disclosed by the invention has the advantages of higher mechanical strength, favorable toughness, favorable wear resistance, favorable etching resistance and favorable chemical resistance, and can satisfy various requirements for paints.

Description

A kind of preparation method of modified epoxy
Technical field
The present invention relates to a kind of resin, be specifically related to a kind of preparation method of modified epoxy.
Background technology
The macromolecular compound that contains epoxide group in all molecular structures is referred to as Resins, epoxy.Resins, epoxy after the curing has good physics, chemical property, it has excellent bonding strength to the surface of metal and non-metallic material, dielectric properties are good, the set shrinking percentage is little, the product size good stability, and hardness is high, snappiness is better, to alkali and most of solvent-stable, thereby be widely used in national defence, each department of national economy, make the purposes such as cast, dipping, lamination material, caking agent, coating.
When Resins, epoxy is used as coating raw material, need it to have good mechanical property, chemical resistance, etch resistance and wear resistance, existing Resins, epoxy often satisfies these requirements simultaneously.
Summary of the invention
Goal of the invention: in order to overcome the deficiencies in the prior art, the invention provides a kind of preparation method of modified epoxy.
Technical scheme: for achieving the above object, the preparation method of a kind of modified epoxy provided by the invention, its preparation process comprises the steps:
(1) organic-treating of polynite: be that to add excessive concentration in 7% the polynite aqueous solution be the 12% Trimethyllaurylammonium bromide aqueous solution with concentration, suction filtration behind 80 ℃ of lower stirring reaction 3~4h is washed till without Br with deionized water -, vacuum-drying is ground to permanent quality, crosses 350 mesh sieves and obtains organo montmorillonite;
(2) preparation of polyethers intercalated montmorillonite: be 30% organo montmorillonite with the above-mentioned pretreated concentration that organises, add among the polyethers N-210, at 60 ℃ of lower dispersed with stirring 4h, grind and obtain polyethers intercalated montmorillonite powder;
(3) base polyurethane prepolymer for use as is synthetic: in reactor, be filled with nitrogen, add TDI and polyethers N-210, at 80~85 ℃ of lower stirring reaction 4h, obtain the N-210 base polyurethane prepolymer for use as;
(4) the nano modified polyurethane performed polymer is synthetic: in reactor, be filled with nitrogen, add the polyethers intercalated montmorillonite powder of processing in TDI and the step (2), at 80~85 ℃ of lower stirring reaction 4h, obtain the nano modified polyurethane performed polymer;
(5) epoxide modified body is synthetic: the nano modified polyurethane performed polymer of getting step (4) gained mixes with Resins, epoxy, namely get epoxide modified body at 120~125 ℃ of lower stirring reactions, described nano modified polyurethane performed polymer and Resins, epoxy mass ratio are 1 ︰ (1.8~2.5);
(6) curing molding: be 40 ︰ (1.8~2.5) in mass ratio with epoxide modified body and solidifying agent polymeric amide, the rear injection mould that stirs solidifies at normal temperatures after 30 days and gets final product.
Preferably, described Resins, epoxy is epoxy resin E-44.
Preferably, the mol ratio of amino hydrogen and epoxy group(ing) is 1:1 in the described solidifying agent polymeric amide.
Beneficial effect: the Resins, epoxy of the present invention's preparation, possess higher mechanical strength, excellent in toughness, wear resistance, etch resistance, chemical resistance are arranged again, can satisfy the requirements as coating.
Embodiment
Below in conjunction with embodiment the present invention is further described.
Embodiment 1:
A kind of modified epoxy preparation method, its preparation process comprises the steps:
(1) organic-treating of polynite: be that to add excessive concentration in 7% the polynite aqueous solution be the 12% Trimethyllaurylammonium bromide aqueous solution with concentration, suction filtration behind 80 ℃ of lower stirring reaction 3h is washed till without Br with deionized water -, vacuum-drying is ground to permanent quality, crosses 350 mesh sieves and obtains organo montmorillonite;
(2) preparation of polyethers intercalated montmorillonite: be 30% organo montmorillonite with the above-mentioned pretreated concentration that organises, add among the polyethers N-210, at 60 ℃ of lower dispersed with stirring 4h, grind and obtain polyethers intercalated montmorillonite powder;
(3) base polyurethane prepolymer for use as is synthetic: in reactor, be filled with nitrogen, add TDI and polyethers N-210, at 80~85 ℃ of lower stirring reaction 4h, obtain the N-210 base polyurethane prepolymer for use as;
(4) the nano modified polyurethane performed polymer is synthetic: in reactor, be filled with nitrogen, add the polyethers intercalated montmorillonite powder of processing in TDI and the step (2), at 80~85 ℃ of lower stirring reaction 4h, obtain the nano modified polyurethane performed polymer;
(5) epoxide modified body is synthetic: the nano modified polyurethane performed polymer of getting step (4) gained mixes with epoxy resin E-44, namely get epoxide modified body at 120~125 ℃ of lower stirring reactions, described nano modified polyurethane performed polymer and Resins, epoxy mass ratio are 1 ︰ 1.8;
(6) curing molding: be 40 ︰ 1.8 in mass ratio with epoxide modified body and solidifying agent polymeric amide, the mol ratio of amino hydrogen and epoxy group(ing) is 1:1 in the solidifying agent polymeric amide, and the rear injection mould that stirs solidifies at normal temperatures after 30 days and gets final product.
Embodiment 2:
A kind of preparation method of modified epoxy is characterized in that: its preparation process comprises the steps:
(1) organic-treating of polynite: be that to add excessive concentration in 7% the polynite aqueous solution be the 12% Trimethyllaurylammonium bromide aqueous solution with concentration, suction filtration behind 80 ℃ of lower stirring reaction 4h is washed till without Br with deionized water -, vacuum-drying is ground to permanent quality, crosses 350 mesh sieves and obtains organo montmorillonite;
(2) preparation of polyethers intercalated montmorillonite: be 30% organo montmorillonite with the above-mentioned pretreated concentration that organises, add among the polyethers N-210, at 60 ℃ of lower dispersed with stirring 4h, grind and obtain polyethers intercalated montmorillonite powder;
(3) base polyurethane prepolymer for use as is synthetic: in reactor, be filled with nitrogen, add TDI and polyethers N-210, at 80~85 ℃ of lower stirring reaction 4h, obtain the N-210 base polyurethane prepolymer for use as;
(4) the nano modified polyurethane performed polymer is synthetic: in reactor, be filled with nitrogen, add the polyethers intercalated montmorillonite powder of processing in TDI and the step (2), at 80~85 ℃ of lower stirring reaction 4h, obtain the nano modified polyurethane performed polymer;
(5) epoxide modified body is synthetic: the nano modified polyurethane performed polymer of getting step (4) gained mixes with Resins, epoxy, namely get epoxide modified body at 120~125 ℃ of lower stirring reactions, described nano modified polyurethane performed polymer and Resins, epoxy mass ratio are 1 ︰ 2.5;
(6) curing molding: be 40 ︰ 2.5 in mass ratio with epoxide modified body and solidifying agent polymeric amide, the mol ratio of amino hydrogen and epoxy group(ing) is 1:1 in the solidifying agent polymeric amide, and the rear injection mould that stirs solidifies at normal temperatures after 30 days and gets final product.
Embodiment 3:
A kind of preparation method of modified epoxy, its preparation process comprises the steps:
(1) organic-treating of polynite: be that to add excessive concentration in 7% the polynite aqueous solution be the 12% Trimethyllaurylammonium bromide aqueous solution with concentration, suction filtration behind 80 ℃ of lower stirring reaction 3~4h is washed till without Br with deionized water -, vacuum-drying is ground to permanent quality, crosses 350 mesh sieves and obtains organo montmorillonite;
(2) preparation of polyethers intercalated montmorillonite: be 30% organo montmorillonite with the above-mentioned pretreated concentration that organises, add among the polyethers N-210, at 60 ℃ of lower dispersed with stirring 4h, grind and obtain polyethers intercalated montmorillonite powder;
(3) base polyurethane prepolymer for use as is synthetic: in reactor, be filled with nitrogen, add TDI and polyethers N-210, at 80~85 ℃ of lower stirring reaction 4h, obtain the N-210 base polyurethane prepolymer for use as;
(4) the nano modified polyurethane performed polymer is synthetic: in reactor, be filled with nitrogen, add the polyethers intercalated montmorillonite powder of processing in TDI and the step (2), at 80~85 ℃ of lower stirring reaction 4h, obtain the nano modified polyurethane performed polymer;
(5) epoxide modified body is synthetic: the nano modified polyurethane performed polymer of getting step (4) gained mixes with epoxy resin E-44, namely get epoxide modified body at 120~125 ℃ of lower stirring reactions, described nano modified polyurethane performed polymer and Resins, epoxy mass ratio are 1 ︰ 2.2;
(6) curing molding: be 40 ︰ 2.3 in mass ratio with epoxide modified body and solidifying agent polymeric amide, the mol ratio of amino hydrogen and epoxy group(ing) is 1:1 in the solidifying agent polymeric amide, and the rear injection mould that stirs solidifies at normal temperatures after 30 days and gets final product.
Among the embodiment 1~3, prepared product performance see the following form:
The above only is preferred implementation of the present invention; be noted that for those skilled in the art; under the prerequisite that does not break away from the principle of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (3)

1. the preparation method of a modified epoxy, it is characterized in that: its preparation process comprises the steps:
(1) organic-treating of polynite: be that to add excessive concentration in 7% the polynite aqueous solution be the 12% Trimethyllaurylammonium bromide aqueous solution with concentration, suction filtration behind 80 ℃ of lower stirring reaction 3~4h is washed till without Br with deionized water -, vacuum-drying is ground to permanent quality, crosses 350 mesh sieves and obtains organo montmorillonite;
(2) preparation of polyethers intercalated montmorillonite: be 30% organo montmorillonite with the above-mentioned pretreated concentration that organises, add among the polyethers N-210, at 60 ℃ of lower dispersed with stirring 4h, grind and obtain polyethers intercalated montmorillonite powder;
(3) base polyurethane prepolymer for use as is synthetic: in reactor, be filled with nitrogen, add TDI and polyethers N-210, at 80~85 ℃ of lower stirring reaction 4h, obtain the N-210 base polyurethane prepolymer for use as;
(4) the nano modified polyurethane performed polymer is synthetic: in reactor, be filled with nitrogen, add the polyethers intercalated montmorillonite powder of processing in TDI and the step (2), at 80~85 ℃ of lower stirring reaction 4h, obtain the nano modified polyurethane performed polymer;
(5) epoxide modified body is synthetic: the nano modified polyurethane performed polymer of getting step (4) gained mixes with Resins, epoxy, namely get epoxide modified body at 120~125 ℃ of lower stirring reactions, described nano modified polyurethane performed polymer and Resins, epoxy mass ratio are 1 ︰ (1.8~2.5);
(6) curing molding: be 40 ︰ (1.8~2.5) in mass ratio with epoxide modified body and solidifying agent polymeric amide, the rear injection mould that stirs solidifies at normal temperatures after 30 days and gets final product.
2. the preparation method of a kind of modified epoxy according to claim 1, it is characterized in that: described Resins, epoxy is epoxy resin E-44.
3. the preparation method of a kind of modified epoxy according to claim 1 is characterized in that:
The mol ratio of amino hydrogen and epoxy group(ing) is 1:1 in the described solidifying agent polymeric amide.
CN2013102733943A 2013-06-28 2013-06-28 Preparation method of modified epoxy resin Pending CN103374115A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103555248A (en) * 2013-11-07 2014-02-05 包兰珍 Modified epoxy resin adhesive and preparation method thereof
CN107254162A (en) * 2017-08-02 2017-10-17 合肥市大卓电力有限责任公司 A kind of cable material with high flame retardant
CN111019100A (en) * 2018-10-10 2020-04-17 中国石油化工股份有限公司 Montmorillonite-modified barrier polyester and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101245223A (en) * 2008-03-17 2008-08-20 四川奥海体育工程有限公司 Environment protection type polyurethane non-particle spray coating material for play ground layer and manufacture method thereof
CN101358031A (en) * 2008-09-08 2009-02-04 南京有志运动场地铺设有限公司 Environment-friendly type paving material for sports field and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101245223A (en) * 2008-03-17 2008-08-20 四川奥海体育工程有限公司 Environment protection type polyurethane non-particle spray coating material for play ground layer and manufacture method thereof
CN101358031A (en) * 2008-09-08 2009-02-04 南京有志运动场地铺设有限公司 Environment-friendly type paving material for sports field and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
申德妍等: ""纳米插层聚氨酯改性环氧树脂性能研究"", 《聚氨酯工业》, vol. 20, no. 3, 28 June 2005 (2005-06-28) *
申德妍等: ""纳米蒙脱土插层聚氨酯改性环氧树脂彩色地坪涂料的研制"", 《涂料工业》, vol. 35, no. 8, 1 August 2005 (2005-08-01) *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103555248A (en) * 2013-11-07 2014-02-05 包兰珍 Modified epoxy resin adhesive and preparation method thereof
CN107254162A (en) * 2017-08-02 2017-10-17 合肥市大卓电力有限责任公司 A kind of cable material with high flame retardant
CN111019100A (en) * 2018-10-10 2020-04-17 中国石油化工股份有限公司 Montmorillonite-modified barrier polyester and preparation method thereof

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Application publication date: 20131030