CN104530389A - Composite curing agent used for treating epoxy resin and preparing method of composite curing agent - Google Patents
Composite curing agent used for treating epoxy resin and preparing method of composite curing agent Download PDFInfo
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- CN104530389A CN104530389A CN201510011212.4A CN201510011212A CN104530389A CN 104530389 A CN104530389 A CN 104530389A CN 201510011212 A CN201510011212 A CN 201510011212A CN 104530389 A CN104530389 A CN 104530389A
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Abstract
The invention discloses a composite curing agent used for treating epoxy resin and a preparing method of the composite curing agent. The composite curing agent comprises, by weight, 15-25 parts of phenol, 5-10 parts of mulberry leaf extracts, 20-50 parts of ketimine, 0.2-0.8 part of a turfy soil extract, and 2-8 parts of sodium polyacrylate. By means of the composite curing agent, curing time of the epoxy resin on the surface of a steel material in a moist environment can be effectively shortened, the impact strength of the epoxy resin can be improved, and coatings are not prone to falling.
Description
Technical field
The present invention relates to a kind of solidifying agent, compound solidifying agent particularly relating to the epoxy coating of fast setting steel surface in wet environment and preparation method thereof.
Background technology
Epoxy resin has excellent physical mechanical, electrical insulation capability and operation method flexibly.Epoxy resin ownership thermosetting resin, belongs to network polymer category, is used alone and does not almost have anything to be worth, only have and in use add solidifying agent, and be cured reaction under certain condition, the product of generating network structure, just can show various excellent performance.
Wherein the single-component system that forms of ketoimine type solidifying agent and epoxy resin is by the moisture that absorbs in air or make ketoimine resolve into amine in water, makes epoxy resin cure, therefore Chang Zuowei wet environment or waterborne curing agents.While ketoimine type solidifying agent cured epoxy resin, also improve the water-repellancy of epoxy coating, wear resistance.But its set time is long, after solidification, resistance to impact shock is general, and these shortcomings are especially serious on die material, cannot meet the industrial standards of increasingly stringent.
Therefore, prior art need to improve.
Summary of the invention
In order to solve the problem of prior art, the object of the present invention is to provide a kind of compound solidifying agent processing epoxy resin and preparation method thereof, this compound solidifying agent can shorten the set time of die material surface epoxy coating in wet environment, improves its resistance to impact shock simultaneously.
Technical scheme of the present invention is as follows: a kind of compound solidifying agent processing epoxy resin, and wherein, the composition of raw materials of this compound solidifying agent is made up of each component of following parts by weight:
Phenol 15 ~ 25 parts;
Mulberries leaf extract 5 ~ 10 parts;
Ketoimine 20 ~ 50 parts;
Turfy soil extract 0.2 ~ 0.8 part;
Sodium polyacrylate 2 ~ 8 parts;
Phenol is a kind of colourless acicular crystal with special odor, is the important source material of producing resin, sterilant, sanitas and medicine.Be slightly soluble in water under normal temperature, be soluble in organic solvent; When temperature is higher than 65 DEG C, can dissolve each other with arbitrary proportion with water.Phenol is corrosive, and can make local protein sex change after contact, and its solution is stained with available ethanol wash on skin.Phenol exposes and is oxidized by oxygen in atmosphere as quinone and pinkiness.The present invention adopts commercially available phenol.
The preparation process of mulberries leaf extract is as follows: pulverized by mulberries leaf, add the deionized water that quality is 5 ~ 10 times, be placed in 10 ~ 40 DEG C of environment (namely under normal temperature) immersion treatment after 15 ~ 25 hours, adopt rotary shaker at 70 ~ 80 DEG C with the speed of 200 ~ 250 turns/min concussion 30 ~ 60 minutes, filter the moisture that post-heating distills 70% ~ 85%, obtain mulberries leaf extract.
Ketoimine is synthesized by aliphatic polyamine and reactive ketone, in colourless low-viscosity (mobile) liquid.Ketoimine of the present invention is the ketoimine adopting polyether-modified fatty amine compounds and methyl iso-butyl ketone (MIBK) to be obtained by reacting.
Turfy soil organic content (abroad think should more than 50%) more than 30%, quality is soft is easy to fragmentary, proportion 0.7-1.05, many in brown or black, and have flammable and inspiratory, pH value is generally 5.5 ~ 6.5, and the reaction in subacidity, in layered distribution.Turfy soil extract preparation process is as follows: pulverized by turfy soil, add the dehydrated alcohol of its material mol ratio 1:3, soak after 30 ~ 40 minutes, adopt rotary shaker to shake 45 ~ 70 minutes with the speed of 180 ~ 230 turns/min at 10 ~ 20 DEG C, filter out large volume impurity, add the deionized water of its quality 3 ~ 5 times, after abundant mixing, leave standstill 100 ~ 120 minutes, siphon supernatant liquid, obtain turfy soil extracting solution.
Sodium polyacrylate is a kind of new functional macromolecule material, and solid product is white (or light yellow) bulk or powder, and liquid product is colourless (or faint yellow) thick liquid, and stablize temperature variation, the aqueous solution has very high viscosity.Viscosity is about the 15-20 of CMC, sodium alginate etc. doubly.According to the different concns of solution and with change pH values such as acetic acid, can adjust the viscosity of its aqueous solution, thermostability is strong, and at 200 DEG C, the divalent-metal ion such as water of decomposition solution and iron, calcium, magnesium combines hardly, forms water-fast gel.Sodium polyacrylate of the present invention adopts commercially available technical grade liquid product.
Contriver is by the experimental study to above-mentioned substance, find the mixing of phenol, mulberries leaf extract and ketoimine, again through treatment process of the present invention, organic molecule in the mixed system obtained is more active, there is good associativity, coordinate certain environmental stress, effectively can shorten the set time of epoxy resin in wet environment.But contriver finds that the resistance to impact shock that this mixed system is processing the coating that epoxy resin obtains is very poor, is significantly less than the solidification effect of ketimine cured dose.So, contriver continues how to improve epoxy coating resistance to impact shock to this mixed system and studies, find this mixed system add sodium polyacrylate comparatively can significantly improve solidification after the resistance to impact shock effect of epoxy resin, contriver's conjecture may be the cohesiveness that has after art breading of sodium polyacrylate and adsorptivity generation effect.And then contriver studies the cohesiveness and adsorptivity that how to improve sodium polyacrylate again, finally find that turfy soil extract polypropylene acid sodium can effectively improve its cohesiveness and adsorptivity.So, above-mentioned substance mixes by contriver, after preparation method's preparation of the present invention, by the compound solidifying agent that obtains for the treatment of epoxy resin, after test repeatedly, obtain a kind of can shorten epoxy resin die material surface set time, improve the solidifying agent of its resistance to impact shock.
Contriver continues to screen the concrete content of each component and test, and finally obtains the component proportion of best results:
Phenol 19 parts;
Mulberries leaf extract 8 parts;
Ketoimine 42 parts;
Turfy soil extract 0.5 part;
Sodium polyacrylate 4.5 parts;
The invention also discloses the preparation method of this compound solidifying agent, comprise the following steps:
First by phenol and ketoimine mixing, stir heated sealed after 30 minutes, Heating temperature maintains 40 ~ 50 DEG C, heat-up time is 10 ~ 20 minutes; Add mulberries leaf extract after placing normal temperature, leave standstill 60 ~ 80 minutes after stirring, obtain mixture A; By turfy soil extract and sodium polyacrylate mixing, add 3 ~ 5 times to the deionized water of its quality, adopt rotary shaker to shake 80 ~ 100 minutes with the speed of 200 ~ 250 turns/min at 50 ~ 70 DEG C, after placing normal temperature, obtain mixture B; Mixture A, B are mixed, adds the deionized water of 2 ~ 4 times of quality after mixing, stir after 30 minutes, with Rotary Evaporators with 40 DEG C ~ 60 DEG C process, until liquid volume reduces 30% ~ 60%, obtain compound solidifying agent.
Beneficial effect of the present invention: compound solidifying agent provided by the invention, effectively can shorten the set time of die material surface epoxy coating in wet environment, improve its resistance to impact shock simultaneously.
Embodiment
For making object of the present invention, technical scheme and advantage clearly, clearly, the present invention is described in more detail below to enumerate embodiment.
Embodiment 1
In the present embodiment, the composition of raw materials of compound ketimine cured dose is made up of each component of following parts by weight:
Phenol 15 parts;
Mulberries leaf extract 5 parts;
Ketoimine 20 parts;
Turfy soil extract 0.2 part;
Sodium polyacrylate 2 parts;
The preparation process of mulberries leaf extract is as follows: pulverized by mulberries leaf, add the deionized water that quality is 8 times, in under normal temperature, immersion treatment is after 23 hours, rotary shaker is adopted to shake 45 minutes with the speed of 220/min at 70 DEG C, filter the moisture that post-heating distills 80%, obtain mulberries leaf extract.
Ketoimine is the ketoimine adopting polyether-modified fatty amine compounds and methyl iso-butyl ketone (MIBK) to be obtained by reacting.
Turfy soil extract preparation process is as follows: pulverized by turfy soil, add the dehydrated alcohol of its material mol ratio 1:3, soak after 30 minutes, adopt rotary shaker to shake 45 minutes with the speed of 180 turns/min at 10 DEG C, filter out large volume impurity, add the deionized water of its quality 3 times, after abundant mixing, leave standstill 100 minutes, siphon supernatant liquid, obtain turfy soil extracting solution.
The preparation method of the compound solidifying agent of the present embodiment is: first by phenol and ketoimine mixing, stir heated sealed after 30 minutes, Heating temperature maintains 40 ~ 50 DEG C, heat-up time is 10 minutes; Add mulberries leaf extract after placing normal temperature, leave standstill 60 minutes after stirring, obtain mixture A; By turfy soil extract and sodium polyacrylate mixing, add 4 times to the deionized water of its quality, adopt rotary shaker to shake 80 minutes with the speed of 220 turns/min at 60 DEG C, after placing normal temperature, obtain mixture B; Mixture A, B are mixed, adds the deionized water of 3 times of quality after mixing, stir after 30 minutes, with Rotary Evaporators with 40 DEG C of process, until liquid volume reduces 50%, obtain compound solidifying agent.
Embodiment 2
In the present embodiment, the composition of raw materials of compound ketimine cured dose is made up of each component of following parts by weight:
Phenol 25 parts;
Mulberries leaf extract 10 parts;
Ketoimine 50 parts;
Turfy soil extract 0.8 part;
Sodium polyacrylate 8 parts;
In the present embodiment, mulberries leaf extract is identical with embodiment 1 with the preparation method of turfy soil extract, ketoimine is the ketoimine adopting polyether-modified fatty amine compounds and methyl iso-butyl ketone (MIBK) to be obtained by reacting, and the preparation method of the compound solidifying agent of the present embodiment is identical with embodiment 1 simultaneously.
Embodiment 3
In the present embodiment, the composition of raw materials of compound ketimine cured dose is made up of each component of following parts by weight:
Phenol 19 parts;
Mulberries leaf extract 8 parts;
Ketoimine 42 parts;
Turfy soil extract 0.5 part;
Sodium polyacrylate 4.5 parts;
Wherein, the preparation process of mulberries leaf extract is as follows: pulverized by mulberries leaf, add the deionized water that quality is 7 times, in under normal temperature, immersion treatment is after 18 hours, rotary shaker is adopted to shake 35 minutes with the speed of 240/min at 75 DEG C, filter the moisture that post-heating distills 75%, obtain mulberries leaf extract.
Ketoimine is the ketoimine adopting polyether-modified fatty amine compounds and methyl iso-butyl ketone (MIBK) to be obtained by reacting.
Turfy soil extract preparation process is as follows: pulverized by turfy soil, add the dehydrated alcohol of its material mol ratio 1:3, soak after 35 minutes, adopt rotary shaker to shake 60 minutes with the speed of 220 turns/min at 20 DEG C, filter out large volume impurity, add the deionized water of its quality 4 times, after abundant mixing, leave standstill 110 minutes, siphon supernatant liquid, obtain turfy soil extracting solution.
The preparation method of the compound solidifying agent of the present embodiment is: first by phenol and ketoimine mixing, stir heated sealed after 30 minutes, Heating temperature maintains 40 ~ 50 DEG C, heat-up time is 15 minutes; Add mulberries leaf extract after placing normal temperature, leave standstill 70 minutes after stirring, obtain mixture A; By turfy soil extract and sodium polyacrylate mixing, add 5 times to the deionized water of its quality, adopt rotary shaker to shake 90 minutes with the speed of 250 turns/min at 55 DEG C, after placing normal temperature, obtain mixture B; Mixture A, B are mixed, adds the deionized water of 4 times of quality after mixing, stir after 30 minutes, with Rotary Evaporators with 50 DEG C of process, until liquid volume reduces 60%, obtain compound solidifying agent.
Comparative example 1
In the present embodiment, the composition of raw materials of compound ketimine cured dose is made up of each component of following parts by weight:
Phenol 15 parts;
Mulberries leaf extract 5 parts;
Ketoimine 20 parts;
Wherein, the preparation method of mulberries leaf extract is identical with embodiment 1, and ketoimine is the ketoimine adopting polyether-modified fatty amine compounds and methyl iso-butyl ketone (MIBK) to be obtained by reacting.
The preparation method of the compound solidifying agent of this comparative example is as follows: first by phenol and ketoimine mixing, stir heated sealed after 30 minutes, Heating temperature maintains 40 ~ 50 DEG C, heat-up time is 10 minutes; Add mulberries leaf extract after placing normal temperature, after stirring, leave standstill 60 minutes, obtain contrasting solidifying agent 1.
Comparative example 2
In the present embodiment, the composition of raw materials of compound ketimine cured dose is made up of each component of following parts by weight:
Phenol 15 parts;
Mulberries leaf extract 5 parts;
Ketoimine 20 parts;
Sodium polyacrylate 2 parts;
Wherein, the preparation method of mulberries leaf extract is identical with embodiment 1, and ketoimine is the ketoimine adopting polyether-modified fatty amine compounds and methyl iso-butyl ketone (MIBK) to be obtained by reacting.
The preparation method of the compound solidifying agent of this comparative example is as follows: first by phenol and ketoimine mixing, stir heated sealed after 30 minutes, Heating temperature maintains 40 ~ 50 DEG C, heat-up time is 10 minutes; Add mulberries leaf extract after placing normal temperature, leave standstill 60 minutes after stirring, obtain mixture A; Sodium polyacrylate is added 4 times to the deionized water of its quality, adopt rotary shaker to shake 80 minutes with the speed of 220 turns/min at 60 DEG C, after placing normal temperature, obtain sodium polyacrylate treatment solution; By mixture A, the mixing of sodium polyacrylate treatment solution, add the deionized water of 3 times of quality after mixing, stir after 30 minutes, with Rotary Evaporators with 40 DEG C of process, until liquid volume reduces 50%, obtain contrasting solidifying agent 2.
Below, application testing experiment is carried out to the even toughener obtained by the various embodiments described above.
1. sample preparation.
After by compound solidifying agent obtained to embodiment 1 ~ 3, comparative example 1 and 2,1:1 mixes in molar ratio with epoxy resin, be applied on 5 block plates respectively, coating thickness is 4mm, the each 20cm of length and width, being positioned over temperature is that 25 DEG C (normal temperature), relative air humidity 90%(are moist) environment in, obtain sample 1 ~ 5;
Adopt commercially available ketimine cured dose, after mixing with epoxy resin by its usage ratio, be applied on the 6th block plate, thickness is 4mm, the each 20cm of length and width, being positioned over temperature is that 25 DEG C (normal temperature), relative air humidity 90%(are moist) environment in, obtain sample 6.
Wherein, sample 1 ~ 6 steel plate used is the shaped steel of same batch, and model specification is consistent; Epoxy resin used is the same batch products that Henan Chi Ao commerce and trade company limited produces.
2. pair sample carries out test experiments, and record data.
Test 2.1 set times
Observation test is carried out to sample 1 ~ 6, and carries out repeating experiment for 10 times and obtain following data form
Upper table can be found out, the average curing time of 1 ~ No. 5 sample is all far smaller than the average curing time of sample 6, and wherein sample 3 solidifies required shortest time.
Test result analysis: by test, can find that the set time of 1 ~ No. 5 sample is significantly less than the set time of sample 6, wherein to solidify required time the shortest for sample 3.
2.2 resistance to impact shock tests
Testing method: adopt falling ball impact test machine, sample is fixedly placed on test table top, by the steel ball of 64g standard from eminence free-electron model on product, falling height is successively increased to 2m with 5cm distance from 20cm, falling height precision is 1mm, the performance of sample for reference and various aspects of performance.Obtain following list data
| Sample number | Test result |
| 1 | Steel ball height rises to 2m, and coating, without distortion, has no coating shedding |
| 2 | Steel ball height rises to 2m, and coating, without distortion, has no coating shedding |
| 3 | Steel ball height rises to 2m, and coating, without distortion, has no coating shedding |
| 4 | Steel ball height rises to 1.45m, and distortion appears in coating; Highly rise to 1.7m, occur obscission; Highly rising to 2m, there is severe detachment in coating |
| 5 | Steel ball height rises to 1.8m, and distortion appears in coating; Highly rise to 2m, occur coming off on a small quantity; |
| 6 | Steel ball height rises to 1.6m, and distortion appears in coating; Highly rise to 1.9m, occur coming off; Highly rise to 2m, occur coming off in a large number |
Test result analysis: have testing data known, the resistance to impact shock of sample 1 ~ 3 is apparently higher than sample 5, and the resistance to impact shock of sample 5 is better than sample 6, and the resistance to impact shock of sample 4 is the poorest.
3. experimental summary: compound solidifying agent provided by the invention effectively can shorten the set time of the epoxy resin of steel surface in wet environment, can improve its resistance to impact shock simultaneously, make coating difficult drop-off.
Should be understood that, application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (3)
1. process a compound solidifying agent for epoxy resin, it is characterized in that, the composition of raw materials of this compound solidifying agent is made up of each component of following parts by weight:
Phenol 15 ~ 25 parts;
Mulberries leaf extract 5 ~ 10 parts;
Ketoimine 20 ~ 50 parts;
Turfy soil extract 0.2 ~ 0.8 part;
Sodium polyacrylate 2 ~ 8 parts;
The preparation process of described mulberries leaf extract is as follows: pulverized by mulberries leaf, add the deionized water that quality is 5 ~ 10 times, be placed in 10 ~ 40 DEG C of environment immersion treatment after 15 ~ 25 hours, adopt rotary shaker at 70 ~ 80 DEG C with the speed of 200 ~ 250 turns/min concussion 30 ~ 60 minutes, filter the moisture that post-heating distills 70% ~ 85%, obtain mulberries leaf extract;
Described turfy soil extract preparation process is as follows: pulverized by turfy soil, add the dehydrated alcohol of its material mol ratio 1:3, soak after 30 ~ 40 minutes, adopt rotary shaker to shake 45 ~ 70 minutes with the speed of 180 ~ 230 turns/min at 10 ~ 20 DEG C, filter out impurity, add the deionized water of its quality 3 ~ 5 times, after abundant mixing, leave standstill 100 ~ 120 minutes, siphon supernatant liquid, obtain turfy soil extracting solution;
Described ketoimine is synthesized by aliphatic polyamine and reactive ketone.
2. the compound solidifying agent of process epoxy resin according to claim 1, is characterized in that, the composition of raw materials of this compound solidifying agent is made up of each component of following parts by weight:
Phenol 19 parts;
Mulberries leaf extract 8 parts;
Ketoimine 42 parts;
Turfy soil extract 0.5 part;
Sodium polyacrylate 4.5 parts.
3. a preparation method for the compound solidifying agent of the process epoxy resin described in claim 1 or 2, is characterized in that, this preparation method comprises the following steps:
First by phenol and ketoimine mixing, stir heated sealed after 30 minutes, Heating temperature maintains 40 ~ 50 DEG C, heat-up time is 10 ~ 20 minutes; Add mulberries leaf extract after placing normal temperature, leave standstill 60 ~ 80 minutes after stirring, obtain mixture A; By turfy soil extract and sodium polyacrylate mixing, add 3 ~ 5 times to the deionized water of its quality, adopt rotary shaker to shake 80 ~ 100 minutes with the speed of 200 ~ 250 turns/min at 50 ~ 70 DEG C, after placing normal temperature, obtain mixture B; Mixture A, B are mixed, adds the deionized water of 2 ~ 4 times of quality after mixing, stir after 30 minutes, with Rotary Evaporators with 40 DEG C ~ 60 DEG C process, until liquid volume reduces 30% ~ 60%, obtain compound solidifying agent.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1576316A (en) * | 2003-07-09 | 2005-02-09 | 气体产品与化学公司 | Epoxy resin compositions |
| CN101885832A (en) * | 2010-07-12 | 2010-11-17 | 中科院广州化灌工程有限公司 | Preparation and application of latent nonionic self-emulsifying epoxy curing agent |
| JP2011116854A (en) * | 2009-12-03 | 2011-06-16 | Adeka Corp | Liquid amine-based latent hardener composition |
| CN103602301A (en) * | 2013-12-03 | 2014-02-26 | 天津市建筑科学研究院有限公司 | Underwater high polymer adhesive and preparation method thereof |
-
2015
- 2015-01-09 CN CN201510011212.4A patent/CN104530389A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1576316A (en) * | 2003-07-09 | 2005-02-09 | 气体产品与化学公司 | Epoxy resin compositions |
| JP2011116854A (en) * | 2009-12-03 | 2011-06-16 | Adeka Corp | Liquid amine-based latent hardener composition |
| CN101885832A (en) * | 2010-07-12 | 2010-11-17 | 中科院广州化灌工程有限公司 | Preparation and application of latent nonionic self-emulsifying epoxy curing agent |
| CN103602301A (en) * | 2013-12-03 | 2014-02-26 | 天津市建筑科学研究院有限公司 | Underwater high polymer adhesive and preparation method thereof |
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Application publication date: 20150422 |