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CN104987654A - Preparation method of phenolic resin composite material for storage tank - Google Patents

Preparation method of phenolic resin composite material for storage tank Download PDF

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Publication number
CN104987654A
CN104987654A CN201510305532.0A CN201510305532A CN104987654A CN 104987654 A CN104987654 A CN 104987654A CN 201510305532 A CN201510305532 A CN 201510305532A CN 104987654 A CN104987654 A CN 104987654A
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phenolic resin
storage tank
resin composite
preparation
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CN104987654B (en
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黄文成
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HEBEI AOKE ZHONGYI ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd.
QINGDAO ACCU GAUGE INSTRUMENT Co.,Ltd.
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Suzhou Zhenzhan Technology Material Co Ltd
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Abstract

The invention provides a preparation method of a phenolic resin composite material for a storage tank. The method comprises the steps that 1, microcrystalline cellulose is dissolved in ionic liquid, the mixture is placed in water bath to be stirred, a cellulose solution is obtained, butyric anhydride is added into the cellulose solution to conduct the reaction, acetic anhydride is added to conduct the reaction continuously, extracting, sedimentation, washing and drying are conducted, and cellulose acetate butyrate is obtained; 2, a coupling agent is dissolved in ethanol, nano-silica is added into an ethanol solution with the coupling agent and taken out for drying, and modified nano-silica is obtained; 3, phenolic resin is dissolved in dimethyl sulfoxide, curing agents, curing catalysts, release agents, toughening agents, glass fibers, the cellulose acetate butyrate and the modified nano-silica are added into the dimethyl sulfoxide with the phenolic resin, ultrasonic agitation and vacuum defoamation are conducted, and a mixture is obtained; 4, the mixture is poured into a mold, after solidification is completed, the mixture is naturally cooled to a room temperature, and the composite material is obtained by taking the material out of the mold. According to the preparation method of the phenolic resin composite material for the storage tank, the composite material is better in low temperature resistance and better in basic performance at low temperatures.

Description

For the preparation method of the phenolic resin composite of storage tank
Technical field:
The present invention relates to phenolic resin composite, particularly relate to the preparation method of the phenolic resin composite for storage tank.
Background technology:
Resol is the resin that phenolic compound and aldehyde compound polycondensation obtain, and the resol wherein obtained with phenol and formaldehyde condensation polymer is the most important.Resol is a kind of the most ancient resin of synthetic, has the use history of last 100 years.Phenolic resin starting material is easy to get, cheap, production technique and equipment simple, and goods have excellent mechanical property, thermotolerance, electrical insulating property, dimensional stability, molding processibility, flame retardant resistance and low smoke, therefore it becomes the indispensable material of industrial sector, and tool has been widely used.Also a lot of occasion is applied to, such as storage tank, pipeline etc. as the matrix material of matrix by resol.
Such as, publication number is CN103113718, publication date is 2013.05.22, apply for that the Chinese patent of artificial China energy construction group Shanxi Electric Power Exploration & Design Institute discloses " a kind of high-strength heat-insulation novolac epoxy composition ", with 100 parts by weight, containing following material: 60-80 part novolac epoxy, 15-30 part glass fibre, 2-4 part microporous calcium silicate, 1-3 part solidifying agent, 1-3 part promotor, this invention has high strength and heat-proof quality, can effectively stop and reduce the generation of storage tank for heat bridge during heat accumulation and elephant.But storage tank also has for the low temperature even occasion of very low temperature, and when being applied to this situation, the described compositions table of this invention is not very desirable with the low-temperature flexibility gone out, and the mechanical properties decrease under low temperature is relatively more serious, and resistance to low temperature is not good.
Summary of the invention:
The technical problem to be solved in the present invention is to provide a kind of preparation method of the phenolic resin composite for storage tank, and the matrix material prepared has good resistance to low temperature, and fundamental property is under cryogenic better.
For solving the problems of the technologies described above, technical scheme of the present invention is:
For a preparation method for the phenolic resin composite of storage tank, its step is as follows:
(1) Microcrystalline Cellulose is dissolved in ionic liquid, be placed in stirred in water bath to dissolve completely to Microcrystalline Cellulose, obtain cellulose solution, butyryl oxide is added in cellulose solution and react 1 hour, add diacetyl oxide and continue reaction 2 hours, whole reaction process stirs and continues to carry out, and extracts product with methylalcohol precipitation, washing 3 times, dry 20 hours in vacuum drying oven, obtain cellulose acetate butyrate;
(2) coupling agent being dissolved in the ethanolic soln that ethanol obtains coupling agent, by adding the ethanolic soln of coupling agent after nano silicon drying and dewatering, heating while stirring, take out after 3 hours and dry, obtain modified manometer silicon dioxide;
(3) by phenol formaldehyde resin dissolves in dimethyl sulfoxide (DMSO), add solidifying agent simultaneously, modified manometer silicon dioxide that cellulose acetate butyrate that curing catalyst, releasing agent, toughner, glass, step (1) obtain, step (2) obtain, the deaeration of ultrasonic agitation final vacuum, obtains compound;
(4) pour the compound that step (3) obtains into mould, mould is put into baking oven and solidifies, after having solidified, naturally cool to room temperature, after feeding, obtain the phenolic resin composite for storage tank.
Preferably, in step of the present invention (1), the mol ratio of Microcrystalline Cellulose, butyryl oxide, diacetyl oxide is 1:4:4.
Preferably, in step of the present invention (1), the temperature of water-bath is 85 DEG C.
Preferably, in step of the present invention (1), the temperature of oven dry is 80 DEG C.
Preferably, in step of the present invention (2), the weight ratio of coupling agent and nano silicon is 1:10.
Preferably, in step of the present invention (2), temperature when heating while stirring is 65 DEG C.
Preferably, in step of the present invention (3), the parts by weight of resol, solidifying agent, curing catalyst, releasing agent, toughner, glass, cellulose acetate butyrate, modified manometer silicon dioxide are respectively 50-60 part, 5-10 part, 2-4 part, 0.5-1 part, 0.1-0.8 part, 10-15 part, 4-9 part, 3-8 part.
Preferably, in step of the present invention (3), the time of ultrasonic agitation is 5 hours.
Preferably, in step of the present invention (3), the time of vacuum defoamation is 1.5 hours.
Preferably, in step of the present invention (4), first solidify 3 hours at 90 DEG C during solidification, then solidify 2 hours at 190 DEG C.
With with have technology with than, the present invention has following beneficial effect:
Cellulose acetate butyrate has good resin and capacitive and winter hardiness, can be dispersed in resin matrix and to produce good interface binding power with resin matrix, thus effectively improving the resistance to low temperature of matrix material; Nano silicon has good mechanical property and thermostability, and specific surface area is comparatively large, surfactivity is strong, bonding action can be played with the group in resin matrix after coupling agent modified, improve Intermolecular Forces, in addition boundary strength is added after nano-silicon dioxide modified, can be dispersed in resin matrix, thus enhancement can be played and improve the thermostability of matrix material, make matrix material still can keep good fundamental property under cryogenic.
Embodiment:
Describe the present invention in detail below in conjunction with specific embodiment, be used for explaining the present invention in this illustrative examples of the present invention and explanation, but not as a limitation of the invention.
Embodiment 1
For the preparation method of the phenolic resin composite of storage tank, its step is as follows:
(1) Microcrystalline Cellulose is dissolved in ionic liquid, be placed in 85 DEG C of stirred in water bath to dissolve completely to Microcrystalline Cellulose, obtain cellulose solution, butyryl oxide is added in cellulose solution and react 1 hour, add diacetyl oxide and continue reaction 2 hours, whole reaction process stirs and continues to carry out, extract product with methylalcohol precipitation, washing 3 times, dry 20 hours at 80 DEG C in vacuum drying oven, obtain cellulose acetate butyrate, wherein, the mol ratio of Microcrystalline Cellulose, butyryl oxide, diacetyl oxide is 1:4:4;
(2) coupling agent is dissolved in the ethanolic soln that ethanol obtains coupling agent, the ethanolic soln of coupling agent will be added after nano silicon drying and dewatering, heat while stirring, temperature during stirring is 65 DEG C, take out after 3 hours and dry, obtain modified manometer silicon dioxide, wherein, the weight ratio of coupling agent and nano silicon is 1:10;
(3) by phenol formaldehyde resin dissolves in dimethyl sulfoxide (DMSO), add solidifying agent simultaneously, curing catalyst, releasing agent, toughner, glass, the cellulose acetate butyrate that step (1) obtains, the modified manometer silicon dioxide that step (2) obtains, ultrasonic agitation final vacuum deaeration in 5 hours 1.5 hours, obtain compound, wherein, resol, solidifying agent, curing catalyst, releasing agent, toughner, glass, cellulose acetate butyrate, the parts by weight of modified manometer silicon dioxide are respectively 50 parts, 6 parts, 2 parts, 0.7 part, 0.4 part, 15 parts, 4 parts, 8 parts,
(4) compound that step (3) obtains is poured into mould, mould is put into baking oven solidify, first solidify 3 hours at 90 DEG C, then solidify 2 hours at 190 DEG C, naturally cool to room temperature after having solidified, after feeding, obtain the phenolic resin composite for storage tank.
Embodiment 2
For the preparation method of the phenolic resin composite of storage tank, its step is as follows:
(1) Microcrystalline Cellulose is dissolved in ionic liquid, be placed in 85 DEG C of stirred in water bath to dissolve completely to Microcrystalline Cellulose, obtain cellulose solution, butyryl oxide is added in cellulose solution and react 1 hour, add diacetyl oxide and continue reaction 2 hours, whole reaction process stirs and continues to carry out, extract product with methylalcohol precipitation, washing 3 times, dry 20 hours at 80 DEG C in vacuum drying oven, obtain cellulose acetate butyrate, wherein, the mol ratio of Microcrystalline Cellulose, butyryl oxide, diacetyl oxide is 1:4:4;
(2) coupling agent is dissolved in the ethanolic soln that ethanol obtains coupling agent, the ethanolic soln of coupling agent will be added after nano silicon drying and dewatering, heat while stirring, temperature during stirring is 65 DEG C, take out after 3 hours and dry, obtain modified manometer silicon dioxide, wherein, the weight ratio of coupling agent and nano silicon is 1:10;
(3) by phenol formaldehyde resin dissolves in dimethyl sulfoxide (DMSO), add solidifying agent simultaneously, curing catalyst, releasing agent, toughner, glass, the cellulose acetate butyrate that step (1) obtains, the modified manometer silicon dioxide that step (2) obtains, ultrasonic agitation final vacuum deaeration in 5 hours 1.5 hours, obtain compound, wherein, resol, solidifying agent, curing catalyst, releasing agent, toughner, glass, cellulose acetate butyrate, the parts by weight of modified manometer silicon dioxide are respectively 54 parts, 9 parts, 2.5 part, 0.9 part, 0.8 part, 14 parts, 7 parts, 4 parts,
(4) compound that step (3) obtains is poured into mould, mould is put into baking oven solidify, first solidify 3 hours at 90 DEG C, then solidify 2 hours at 190 DEG C, naturally cool to room temperature after having solidified, after feeding, obtain the phenolic resin composite for storage tank.
Embodiment 3
For the preparation method of the phenolic resin composite of storage tank, its step is as follows:
(1) Microcrystalline Cellulose is dissolved in ionic liquid, be placed in 85 DEG C of stirred in water bath to dissolve completely to Microcrystalline Cellulose, obtain cellulose solution, butyryl oxide is added in cellulose solution and react 1 hour, add diacetyl oxide and continue reaction 2 hours, whole reaction process stirs and continues to carry out, extract product with methylalcohol precipitation, washing 3 times, dry 20 hours at 80 DEG C in vacuum drying oven, obtain cellulose acetate butyrate, wherein, the mol ratio of Microcrystalline Cellulose, butyryl oxide, diacetyl oxide is 1:4:4;
(2) coupling agent is dissolved in the ethanolic soln that ethanol obtains coupling agent, the ethanolic soln of coupling agent will be added after nano silicon drying and dewatering, heat while stirring, temperature during stirring is 65 DEG C, take out after 3 hours and dry, obtain modified manometer silicon dioxide, wherein, the weight ratio of coupling agent and nano silicon is 1:10;
(3) by phenol formaldehyde resin dissolves in dimethyl sulfoxide (DMSO), add solidifying agent simultaneously, curing catalyst, releasing agent, toughner, glass, the cellulose acetate butyrate that step (1) obtains, the modified manometer silicon dioxide that step (2) obtains, ultrasonic agitation final vacuum deaeration in 5 hours 1.5 hours, obtain compound, wherein, resol, solidifying agent, curing catalyst, releasing agent, toughner, glass, cellulose acetate butyrate, the parts by weight of modified manometer silicon dioxide are respectively 52 parts, 7 parts, 3.5 part, 1 part, 0.6 part, 10 parts, 8 parts, 5 parts,
(4) compound that step (3) obtains is poured into mould, mould is put into baking oven solidify, first solidify 3 hours at 90 DEG C, then solidify 2 hours at 190 DEG C, naturally cool to room temperature after having solidified, after feeding, obtain the phenolic resin composite for storage tank.
Embodiment 4
For the preparation method of the phenolic resin composite of storage tank, its step is as follows:
(1) Microcrystalline Cellulose is dissolved in ionic liquid, be placed in 85 DEG C of stirred in water bath to dissolve completely to Microcrystalline Cellulose, obtain cellulose solution, butyryl oxide is added in cellulose solution and react 1 hour, add diacetyl oxide and continue reaction 2 hours, whole reaction process stirs and continues to carry out, extract product with methylalcohol precipitation, washing 3 times, dry 20 hours at 80 DEG C in vacuum drying oven, obtain cellulose acetate butyrate, wherein, the mol ratio of Microcrystalline Cellulose, butyryl oxide, diacetyl oxide is 1:4:4;
(2) coupling agent is dissolved in the ethanolic soln that ethanol obtains coupling agent, the ethanolic soln of coupling agent will be added after nano silicon drying and dewatering, heat while stirring, temperature during stirring is 65 DEG C, take out after 3 hours and dry, obtain modified manometer silicon dioxide, wherein, the weight ratio of coupling agent and nano silicon is 1:10;
(3) by phenol formaldehyde resin dissolves in dimethyl sulfoxide (DMSO), add solidifying agent simultaneously, curing catalyst, releasing agent, toughner, glass, the cellulose acetate butyrate that step (1) obtains, the modified manometer silicon dioxide that step (2) obtains, ultrasonic agitation final vacuum deaeration in 5 hours 1.5 hours, obtain compound, wherein, resol, solidifying agent, curing catalyst, releasing agent, toughner, glass, cellulose acetate butyrate, the parts by weight of modified manometer silicon dioxide are respectively 60 parts, 8 parts, 4 parts, 0.6 part, 0.7 part, 11 parts, 6 parts, 7 parts,
(4) compound that step (3) obtains is poured into mould, mould is put into baking oven solidify, first solidify 3 hours at 90 DEG C, then solidify 2 hours at 190 DEG C, naturally cool to room temperature after having solidified, after feeding, obtain the phenolic resin composite for storage tank.
Embodiment 5
For the preparation method of the phenolic resin composite of storage tank, its step is as follows:
(1) Microcrystalline Cellulose is dissolved in ionic liquid, be placed in 85 DEG C of stirred in water bath to dissolve completely to Microcrystalline Cellulose, obtain cellulose solution, butyryl oxide is added in cellulose solution and react 1 hour, add diacetyl oxide and continue reaction 2 hours, whole reaction process stirs and continues to carry out, extract product with methylalcohol precipitation, washing 3 times, dry 20 hours at 80 DEG C in vacuum drying oven, obtain cellulose acetate butyrate, wherein, the mol ratio of Microcrystalline Cellulose, butyryl oxide, diacetyl oxide is 1:4:4;
(2) coupling agent is dissolved in the ethanolic soln that ethanol obtains coupling agent, the ethanolic soln of coupling agent will be added after nano silicon drying and dewatering, heat while stirring, temperature during stirring is 65 DEG C, take out after 3 hours and dry, obtain modified manometer silicon dioxide, wherein, the weight ratio of coupling agent and nano silicon is 1:10;
(3) by phenol formaldehyde resin dissolves in dimethyl sulfoxide (DMSO), add solidifying agent simultaneously, curing catalyst, releasing agent, toughner, glass, the cellulose acetate butyrate that step (1) obtains, the modified manometer silicon dioxide that step (2) obtains, ultrasonic agitation final vacuum deaeration in 5 hours 1.5 hours, obtain compound, wherein, resol, solidifying agent, curing catalyst, releasing agent, toughner, glass, cellulose acetate butyrate, the parts by weight of modified manometer silicon dioxide are respectively 56 parts, 10 parts, 3 parts, 0.8 part, 0.5 part, 13 parts, 5 parts, 6 parts,
(4) compound that step (3) obtains is poured into mould, mould is put into baking oven solidify, first solidify 3 hours at 90 DEG C, then solidify 2 hours at 190 DEG C, naturally cool to room temperature after having solidified, after feeding, obtain the phenolic resin composite for storage tank.
Embodiment 6
For the preparation method of the phenolic resin composite of storage tank, its step is as follows:
(1) Microcrystalline Cellulose is dissolved in ionic liquid, be placed in 85 DEG C of stirred in water bath to dissolve completely to Microcrystalline Cellulose, obtain cellulose solution, butyryl oxide is added in cellulose solution and react 1 hour, add diacetyl oxide and continue reaction 2 hours, whole reaction process stirs and continues to carry out, extract product with methylalcohol precipitation, washing 3 times, dry 20 hours at 80 DEG C in vacuum drying oven, obtain cellulose acetate butyrate, wherein, the mol ratio of Microcrystalline Cellulose, butyryl oxide, diacetyl oxide is 1:4:4;
(2) coupling agent is dissolved in the ethanolic soln that ethanol obtains coupling agent, the ethanolic soln of coupling agent will be added after nano silicon drying and dewatering, heat while stirring, temperature during stirring is 65 DEG C, take out after 3 hours and dry, obtain modified manometer silicon dioxide, wherein, the weight ratio of coupling agent and nano silicon is 1:10;
(3) by phenol formaldehyde resin dissolves in dimethyl sulfoxide (DMSO), add solidifying agent simultaneously, curing catalyst, releasing agent, toughner, glass, the cellulose acetate butyrate that step (1) obtains, the modified manometer silicon dioxide that step (2) obtains, ultrasonic agitation final vacuum deaeration in 5 hours 1.5 hours, obtain compound, wherein, resol, solidifying agent, curing catalyst, releasing agent, toughner, glass, cellulose acetate butyrate, the parts by weight of modified manometer silicon dioxide are respectively 57 parts, 5 parts, 4 parts, 0.7 part, 0.1 part, 12 parts, 9 parts, 3 parts,
(4) compound that step (3) obtains is poured into mould, mould is put into baking oven solidify, first solidify 3 hours at 90 DEG C, then solidify 2 hours at 190 DEG C, naturally cool to room temperature after having solidified, after feeding, obtain the phenolic resin composite for storage tank.
After tested, the matrix material that embodiment 1-6 obtains and comparative example mechanical property under cryogenic as shown in the table, the wherein Chinese patent of comparative example to be publication number be CN103113718:
As seen from the above table, the matrix material that the present invention obtains every mechanical property under cryogenic, all significantly better than comparative example, possesses good resistance to low temperature.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.

Claims (10)

1. for the preparation method of the phenolic resin composite of storage tank, it is characterized in that: its step is as follows:
(1) Microcrystalline Cellulose is dissolved in ionic liquid, be placed in stirred in water bath to dissolve completely to Microcrystalline Cellulose, obtain cellulose solution, butyryl oxide is added in cellulose solution and react 1 hour, add diacetyl oxide and continue reaction 2 hours, whole reaction process stirs and continues to carry out, and extracts product with methylalcohol precipitation, washing 3 times, dry 20 hours in vacuum drying oven, obtain cellulose acetate butyrate;
(2) coupling agent being dissolved in the ethanolic soln that ethanol obtains coupling agent, by adding the ethanolic soln of coupling agent after nano silicon drying and dewatering, heating while stirring, take out after 3 hours and dry, obtain modified manometer silicon dioxide;
(3) by phenol formaldehyde resin dissolves in dimethyl sulfoxide (DMSO), add solidifying agent simultaneously, modified manometer silicon dioxide that cellulose acetate butyrate that curing catalyst, releasing agent, toughner, glass, step (1) obtain, step (2) obtain, the deaeration of ultrasonic agitation final vacuum, obtains compound;
(4) pour the compound that step (3) obtains into mould, mould is put into baking oven and solidifies, after having solidified, naturally cool to room temperature, after feeding, obtain the phenolic resin composite for storage tank.
2. the preparation method of the phenolic resin composite for storage tank according to claim 1, is characterized in that: in described step (1), and the mol ratio of Microcrystalline Cellulose, butyryl oxide, diacetyl oxide is 1:4:4.
3. the preparation method of the phenolic resin composite for storage tank according to claim 1, is characterized in that: in described step (1), and the temperature of water-bath is 85 DEG C.
4. the preparation method of the phenolic resin composite for storage tank according to claim 1, is characterized in that: in described step (1), and the temperature of oven dry is 80 DEG C.
5. the preparation method of the phenolic resin composite for storage tank according to claim 1, is characterized in that: in described step (2), and the weight ratio of coupling agent and nano silicon is 1:10.
6. the preparation method of the phenolic resin composite for storage tank according to claim 1, is characterized in that: in described step (2), and temperature when heating while stirring is 65 DEG C.
7. the preparation method of the phenolic resin composite for storage tank according to claim 1, it is characterized in that: in described step (3), the parts by weight of resol, solidifying agent, curing catalyst, releasing agent, toughner, glass, cellulose acetate butyrate, modified manometer silicon dioxide are respectively 50-60 part, 5-10 part, 2-4 part, 0.5-1 part, 0.1-0.8 part, 10-15 part, 4-9 part, 3-8 part.
8. the preparation method of the phenolic resin composite for storage tank according to claim 1, is characterized in that: in described step (3), and the time of ultrasonic agitation is 5 hours.
9. the preparation method of the phenolic resin composite for storage tank according to claim 1, is characterized in that: in described step (3), and the time of vacuum defoamation is 1.5 hours.
10. the preparation method of the phenolic resin composite for storage tank according to claim 1, is characterized in that: in described step (4), first solidifies 3 hours at 90 DEG C during solidification, then solidifies 2 hours at 190 DEG C.
CN201510305532.0A 2015-06-05 2015-06-05 Preparation method for the phenolic resin composite of storage tank Active CN104987654B (en)

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CN106751432A (en) * 2016-12-22 2017-05-31 苏州缔绿电子科技有限公司 A kind of low-temperature-resistance high-toughness composite and preparation method thereof
CN109180210A (en) * 2018-09-12 2019-01-11 中国科学院金属研究所 A kind of method and its application of the interior filling active carbon of prefabricated carbon fiber body

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Cited By (2)

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