CN104877304B - A kind of preparation method of bamboo liquefied phenolic resin sealing end perlite load phase-change material - Google Patents

A kind of preparation method of bamboo liquefied phenolic resin sealing end perlite load phase-change material Download PDF

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CN104877304B
CN104877304B CN201510317093.5A CN201510317093A CN104877304B CN 104877304 B CN104877304 B CN 104877304B CN 201510317093 A CN201510317093 A CN 201510317093A CN 104877304 B CN104877304 B CN 104877304B
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perlite
bamboo
change material
phenolic resin
phase
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CN104877304A (en
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刘乐群
张文福
方晶
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Zhejiang Academy of Forestry
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Zhejiang Academy of Forestry
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Abstract

The invention discloses a kind of preparation methods of bamboo liquefied phenolic resin sealing end perlite load phase-change material, include the following steps:Bamboo surplus material of processing after phenol, polyethylene glycol 400,37% hydrochloric acid and crushing is mixed in proportion, is liquefied to bamboo surplus material of processing, then, adds in 40%NaOH and formaldehyde, obtains bamboo particle liquefaction phenolic resin;After phase-change material is taken to melt, the perlite that grain size is 550 μm 1500 μm, vacuumizing and adsorbing are added in;The resin of above-mentioned gained is taken to be added in the perlite of load phase-change material of above-mentioned gained, when vacuumizing and adsorbing 1 is small;Pickling is carried out to the mixture of gained, after impregnating 10min, is filtered, when vacuumizing and adsorbing 1 is small;The mixture of gained is dried in vacuo, obtains finished product.The present invention makes full use of the characteristic of bamboo liquefied phenolic resin, solves the problems, such as perlite load phase-change material leakage, ensure that the thermal stability of phase-change material.

Description

A kind of preparation method of bamboo liquefied phenolic resin sealing end perlite load phase-change material
Technical field
The present invention relates to biomass energy-storage composite material fields, and in particular to a kind of bamboo liquefied phenolic resin blocks pearl Rock loads the preparation method of phase-change material.
Background technology
China's bamboo resource is very abundant, and bamboo grove area accounts for the world 1/4.Accumulation and the bamboo wood annual output Jun Zhan worlds 1/3, bamboo Material has that growth is fast, becomes a useful person morning, has become one of the important fast-growing in China and renewable forest reserves, common bamboo processing Utilization rate is less than 40%, and most of bamboo wood can generate bamboo particle in process, these bamboo particle parts are used to process bamboo wood Fiberboard largely by discarded burning, recycles added value relatively low.
Bamboo liquefied phenolic resin is made using bamboo particle, is one of effective means that bamboo wood chemical conversion utilizes, the tree Fat not only has the characteristic of phenolic resin, also containing the macromolecular nanoparticles after bamboo liquefied, is uniformly dispersed, and has one Fixed expandability and adhesivity.
Perlite is the silicate melt of multicomponent system, inside be cellular structures, its main feature is that unit weight is light, absolutely Heat and attracting performance are good, have stronger adsorption capacity, and raw material sources enrich, cheap, therefore in phase-change material making, one As can use perlite as carrier, but in the production process, often there is a situation where that phase-change material is revealed.
The content of the invention
To solve the above problems, the present invention provides a kind of bamboo liquefied phenolic resin sealing end perlite load phase-change materials Preparation method, by the way that bamboo particle is chemically converted into liquid, using the distinctive characteristic of bamboo liquefied phenolic resin, one Under the conditions of constant temperature degree and acid value, bamboo liquefied resin can be made to fill perlite micropore, reduce phase-change material in phase transition process In leakage.
To achieve the above object, the technical solution taken of the present invention is:
A kind of preparation method of bamboo liquefied phenolic resin sealing end perlite load phase-change material, includes the following steps:
S1, bamboo processing of the grain size less than 380 microns after phenol, polyethylene glycol-400,37% hydrochloric acid and crushing is remained Excess example 1: 1 in mass ratio:: after 1: 1.5 mixing, liquefy to bamboo surplus material of processing under 120-140 DEG C of temperature conditionss 30- 60min, then, the formaldehyde for adding in the 40%NaOH aqueous solutions of 2.34 times of amounts of phenol usage and 2.37 times of amounts of phenol usage are molten Liquid under the conditions of 80-100 DEG C, heats 45-75min, obtains bamboo particle liquefaction phenolic resin;
S2, after 20-70g phase-change materials is taken to melt, the perlite that 10-15g grain sizes are more than 550-1500 μm is added in, mixing is equal It is even, vacuumizing and adsorbing;
S3, the resin obtained by 10-30g steps S1 is taken to be added in the perlite of the load phase-change material obtained by step S2, Under the conditions of 30-50 DEG C, when vacuumizing and adsorbing 1 is small;
S4, pickling is carried out to the mixture obtained by step S3 using phosphoric acid, after impregnating 10min, filtered, in 30-50 DEG C of item When vacuumizing and adsorbing 1 is small under part;
S5, the mixture obtained by step S4 is dried in vacuo, when drying 10-16 is small, obtains finished product.
Wherein, the phase-change material is organic paraffin class, organic fatty alcohol.
Wherein, organic paraffin class is one kind in paraffin, n-octadecane.
Wherein, the organic fatty alcohol is one kind in hexadecanol, tetradecyl alchohol.
Bamboo crushed aggregates through liquefaction and resinification, are fabricated to bamboo liquefied phenolic resin, which has by this specific implementation It is uniformly dispersed, not only the characteristic with phenolic resin, it, can be preferable also containing the macromolecular nanoparticles after bamboo liquefied Perlite surface is attached to, under the conditions of certain temperature and acid value, is handled by negative pressure of vacuum, perlite micropore can be filled, Preferable cladding perlite, prevents the leakage of the phase-change material of perlite load.
The invention has the advantages that:
The characteristic of bamboo liquefied phenolic resin is made full use of, perlite load phase-change material leakage is solved the problems, such as, protects The thermal stability of phase-change material is demonstrate,proved.
Specific embodiment
In order to which objects and advantages of the present invention are more clearly understood, the present invention is carried out with reference to embodiments further It is described in detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit this hair It is bright.
In following embodiment, phase-change material is organic paraffin class, organic fatty alcohol;Organic paraffin class is paraffin, positive 18 One kind in alkane;Organic fatty alcohol is hexadecanol, one kind in tetradecyl alchohol
Embodiment 1.
S1, bamboo processing of the grain size less than 380 microns after phenol, polyethylene glycol-400,37% hydrochloric acid and crushing is remained Excess example 1: 1 in mass ratio:: after 1: 1.5 mixing, liquefy to bamboo surplus material of processing under 120 DEG C of temperature conditionss 30min, so Afterwards, the formalin of the 40%NaOH aqueous solutions of 2.34 times of amounts of phenol usage and 2.37 times of amounts of phenol usage is added in, 80 Under the conditions of DEG C, 75min is heated, obtains bamboo particle liquefaction phenolic resin;
S2, after 20g phase-change materials is taken to melt, the perlite that 10g grain sizes are more than 550 μm is added in, is uniformly mixed, vacuumizes suction It is attached;
S3, the resin obtained by 10g steps S1 is taken to be added in the perlite of the load phase-change material obtained by step S2,30 Under the conditions of DEG C, when vacuumizing and adsorbing 1 is small;
S4, pickling is carried out to the mixture obtained by step S3 using phosphoric acid, after impregnating 10min, filtered, under the conditions of 30 DEG C When vacuumizing and adsorbing 1 is small;
S5, the mixture obtained by step S4 is dried in vacuo, when drying 10 is small, obtains finished product.
Embodiment 2
S1, bamboo processing of the grain size less than 380 microns after phenol, polyethylene glycol-400,37% hydrochloric acid and crushing is remained Excess example 1: 1 in mass ratio:: after 1: 1.5 mixing, liquefy to bamboo surplus material of processing under 140 DEG C of temperature conditionss 30-60min, Then, the formalin of the 40%NaOH aqueous solutions of 2.34 times of amounts of phenol usage and 2.37 times of amounts of phenol usage is added in, Under the conditions of 100 DEG C, 45min is heated, obtains bamboo particle liquefaction phenolic resin;
S2, after 70g phase-change materials is taken to melt, the perlite that 15g grain sizes are more than 1500 μm is added in, is uniformly mixed, vacuumizes Absorption;
S3, the resin obtained by 10-30g steps S1 is taken to be added in the perlite of the load phase-change material obtained by step S2, Under the conditions of 50 DEG C, when vacuumizing and adsorbing 1 is small;
S4, pickling is carried out to the mixture obtained by step S3 using phosphoric acid, after impregnating 10min, filtered, under the conditions of 50 DEG C When vacuumizing and adsorbing 1 is small;
S5, the mixture obtained by step S4 is dried in vacuo, when drying 16 is small, obtains finished product.
Embodiment 3
S1, bamboo processing of the grain size less than 380 microns after phenol, polyethylene glycol-400,37% hydrochloric acid and crushing is remained Excess example 1: 1 in mass ratio:: after 1: 1.5 mixing, liquefy to bamboo surplus material of processing under 130 DEG C of temperature conditionss 45min, so Afterwards, the formalin of the 40%NaOH aqueous solutions of 2.34 times of amounts of phenol usage and 2.37 times of amounts of phenol usage is added in, 90 Under the conditions of DEG C, 60min is heated, obtains bamboo particle liquefaction phenolic resin;
S2, after 45g phase-change materials is taken to melt, the perlite that 12.5g grain sizes are more than 1025 μm is added in, be uniformly mixed, taken out true Suction is attached;
S3, the resin obtained by 20g steps S1 is taken to be added in the perlite of the load phase-change material obtained by step S2,40 Under the conditions of DEG C, when vacuumizing and adsorbing 1 is small;
S4, pickling is carried out to the mixture obtained by step S3 using phosphoric acid, after impregnating 10min, filtered, under the conditions of 40 DEG C When vacuumizing and adsorbing 1 is small;
S5, the mixture obtained by step S4 is dried in vacuo, when drying 13 is small, obtains finished product
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, without departing from the principle of the present invention, several improvements and modifications can also be made, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (4)

1. a kind of preparation method of bamboo liquefied phenolic resin sealing end perlite load phase-change material, which is characterized in that including such as Lower step:
S1, the bamboo surplus material of processing that the grain size after phenol, polyethylene glycol-400,37% hydrochloric acid and crushing is less than to 380 microns Example 1: 1 in mass ratio:: after 1: 1.5 mixing, liquefy to bamboo surplus material of processing under 120-140 DEG C of temperature conditionss 30-60min, Then, the formalin of the 40%NaOH aqueous solutions of 2.34 times of amounts of phenol usage and 2.37 times of amounts of phenol usage is added in, Under the conditions of 80-100 DEG C, 45-75min is heated, obtains bamboo particle liquefaction phenolic resin;
S2, after 20-70g phase-change materials is taken to melt, the perlite that 10-15g grain sizes are 550 μm -1500 μm is added in, is uniformly mixed, Vacuumizing and adsorbing;
S3, the resin obtained by 10-30g steps S1 is taken to be added in the perlite of the load phase-change material obtained by step S2, in 30- Under the conditions of 50 DEG C, when vacuumizing and adsorbing 1 is small;
S4, pickling is carried out to the mixture obtained by step S3 using phosphoric acid, after impregnating 10min, filtered, under the conditions of 30-50 DEG C When vacuumizing and adsorbing 1 is small;
S5, the mixture obtained by step S4 is dried in vacuo, when drying 10-16 is small, obtains finished product.
2. a kind of preparation side of bamboo liquefied phenolic resin sealing end perlite load phase-change material according to claim 1 Method, which is characterized in that the phase-change material is organic paraffin class, organic fatty alcohol.
3. a kind of preparation side of bamboo liquefied phenolic resin sealing end perlite load phase-change material according to claim 1 Method, which is characterized in that organic paraffin class is paraffin, one kind in n-octadecane.
4. a kind of preparation side of bamboo liquefied phenolic resin sealing end perlite load phase-change material according to claim 1 Method, which is characterized in that the organic fatty alcohol is hexadecanol, one kind in tetradecyl alchohol.
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CN105906257B (en) * 2016-04-03 2017-12-01 黄河水利职业技术学院 A kind of construction material
CN108130046A (en) * 2017-11-29 2018-06-08 贵州省材料产业技术研究院 Paraffin/Heat Conduction Material/polymer hollow fiber membrane composite phase-change material and preparation method thereof can be woven
CN113084393B (en) * 2021-04-21 2022-06-17 兰州理工大学 Antioxidant soldering flux for welding metal materials
CN114950503B (en) * 2021-12-21 2023-08-18 常州市金坛区维格生物科技有限公司 Preparation method and application of regenerated acid catalyst

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CN101096298A (en) * 2006-06-28 2008-01-02 宁波荣山新型材料有限公司 Organic phase-change composite expanding perlite and preparation method thereof
CN101139181A (en) * 2007-07-25 2008-03-12 宁波荣山新型材料有限公司 Process for preparing organic phase-change material composite expanded perlite by emulsification method
CN101348708A (en) * 2008-09-17 2009-01-21 中国建筑材料科学研究总院 Preparation of organic inorganic composite phase-change material
CN104387720A (en) * 2014-10-16 2015-03-04 浙江省林业科学研究院 Perlite added bamboo wood foamed composite material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101096298A (en) * 2006-06-28 2008-01-02 宁波荣山新型材料有限公司 Organic phase-change composite expanding perlite and preparation method thereof
CN101139181A (en) * 2007-07-25 2008-03-12 宁波荣山新型材料有限公司 Process for preparing organic phase-change material composite expanded perlite by emulsification method
CN101348708A (en) * 2008-09-17 2009-01-21 中国建筑材料科学研究总院 Preparation of organic inorganic composite phase-change material
CN104387720A (en) * 2014-10-16 2015-03-04 浙江省林业科学研究院 Perlite added bamboo wood foamed composite material and preparation method thereof

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