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CN107267162B - A kind of preparation method of nanometer attapulgite-based inorganic flame retardant - Google Patents

A kind of preparation method of nanometer attapulgite-based inorganic flame retardant Download PDF

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Publication number
CN107267162B
CN107267162B CN201710580377.2A CN201710580377A CN107267162B CN 107267162 B CN107267162 B CN 107267162B CN 201710580377 A CN201710580377 A CN 201710580377A CN 107267162 B CN107267162 B CN 107267162B
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recessed
auxiliary material
mixing
preparation
soil
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CN107267162A (en
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胡涛
熊清平
石莹莹
谭立强
蒯海伟
张立静
王志辉
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Hebei Xingchen Wood Industry Co Ltd
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Huaiyin Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K21/00Fireproofing materials
    • C09K21/14Macromolecular materials
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K21/00Fireproofing materials
    • C09K21/02Inorganic materials

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Soil Conditioners And Soil-Stabilizing Materials (AREA)

Abstract

本发明公开了一种纳米凹土基无机阻燃剂的制备方法,该纳米凹土基无机阻燃剂的制备方法具体步骤如下:S1:凹土的选材,S2:凹土的搅拌混合,S3:第一辅料的混合加入,S4:静置,S5:过滤处理,S6:二次研磨处理,S7:第二辅料的混合加入。本发明采用凹土的使用可以获得凹土的粘性,同时将凹土的阻燃性能得到有效的利用,充分利用凹土的阻燃性,同时配合其他第一辅料和第二辅料的加入进一步的提高阻燃性能,同时可以获得良好的粘合性能,更加便于使用。The invention discloses a preparation method of a nano attapulgite-based inorganic flame retardant. The specific steps of the preparation method of the nano attapulgite-based inorganic flame retardant are as follows: S1: material selection of attapulgite, S2: stirring and mixing of attapulgite, S3 : mixing and adding of the first auxiliary material, S4: standing still, S5: filtering treatment, S6: secondary grinding treatment, S7: mixing and adding of the second auxiliary material. The invention adopts the use of attapulgite to obtain the viscosity of attapulgite, and at the same time effectively utilizes the flame retardant properties of attapulgite, makes full use of the flame retardancy of attapulgite, and at the same time cooperates with the addition of other first auxiliary materials and second auxiliary materials to further improve the Improve the flame retardant performance, and at the same time obtain good adhesion performance, which is more convenient to use.

Description

A kind of preparation method of nano concave soil base inorganic flame-retarded agent
Technical field
The present invention relates to fire retardant improving technology field, specially a kind of preparation side of nano concave soil base inorganic flame-retarded agent Method.
Background technique
Recessed soil is the abbreviation of attapulgite clay (Attapulgite Clay).It is a kind of rare nonmetal mineral resource, it It is the aqueous rich magnesium aluminosilicate clays mineral of a kind of layer of chain structure.
Recessed soil is as a kind of important scarcity nonmetal mineral resource, in farming and animal husbandry, building materials, petroleum, metallurgy, food etc. 10 multiple fields extensive applications.Concave-convex clay rod is one of China's advantage nonmetallic ore, and purposes is very extensive, is claimed For " thousand with soil, ten thousand soil king ".The ice bag that recessed soil is added still does not freeze in 40 degrees below zero, and steamed bun is placed on recessed soil system At hermetically sealed can in be also able to maintain within 8 months it is fresh, with it is recessed soil made of craftwork can purify air.Recessed soil has sterilizing, removes Smelly, detoxification, pesticidal function.It is such as used for diarrhea, is to adsorb the toadstool in stomach with it;The recessed tiny elongated piece of soil is to insect Surface abrasion and insect lipids is adsorbed, insect quick death and military project is caused to adsorb poison gas for protective device, Absorb animal and vegetable oil pigment, aflatoxins and stink etc..In brewery industry, grape wine, applejack, beer are clarified with recessed soil The drinks product such as wine can remove the various residue impurity in wine, keep vinosity pure.From the point of view of chemical industry, recessed soil has table Face activated centre, in addition to absorption, there are also catalytic action.Recessed soil can be used as the catalyst that ethyl alcohol is converted into ethylene, also can be used as and urges Agent carrier.Meanwhile the Concave-convex clay rod product after processing is ideal adsorbent, food processing aid and food additive Add agent, may replace active carbon.The production composition for the instant noodles that many people eat is useful to it.
It can use the anti-flammability of recessed soil using recessed soil as the matrix of fire retardant, so that recessed soil is effectively utilized, It is simultaneously that we need the problem of facing as the fire retardant exploitation of matrix to recessed soil.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of nano concave soil base inorganic flame-retarded agent, the nano concave earth base without Specific step is as follows for the preparation method of machine fire retardant:
S1: the selection of recessed soil selects recessed soil of the purity higher than 98% to be used as recessed soil matrix, is ground, grinds to recessed soil Sieving processing is carried out after mill, the mesh number of recessed soil powder in 2000-3000 mesh, place spare by the recessed native powder of sieving;
S2: recessed soil is stirred, and according to composition by weight ratio is after 1:5 mixing match in blender by recessed native powder and water In be mixed, at 1200-1500 revs/min, the time of mixing controlled at 30-50 minutes blender revolving speed;
The mixing of S3: the first auxiliary material is added, and continues to be mixed 10-15 minutes after auxiliary material is added, blender revolving speed is 600-800 revs/min, and the mixing after auxiliary material addition uses the mixing of heating type, temperature when heating is mixed Degree is at 80-95 DEG C;
S4: standing, and the material after heating stirring is taken out placement and carries out standing placement in a reservoir, time of repose is at least 3-5 hours;
S5: the solution upper clear supernate after standing is filtered removal, bottom precipitation is taken out, in drying equipment by filtration treatment Middle carry out drying and processing, drying temperature are controlled at 150-180 DEG C, and drying time was at 30-40 minutes;
S6: the material taking-up after drying is carried out secondary milled processed by secondary milled processed in milling apparatus, secondary to grind Treated that powder mesh number takes out after 2000-2500 mesh, grinding is spare for mill;
The mixing of S7: the second auxiliary material is added, and Hybrid Heating stirs after the second auxiliary material is added, and the temperature of heating is in 110- 130 DEG C, cooling processing is carried out after being mixed evenly, the laggard luggage bag of room temperature is cooled to and seals spare, completion nano concave earth base The process of inorganic fire retardants.
Preferably, first auxiliary material to be fire retardant, curing agent and carbon forming agent according to composition by weight ratio be 1:1:1 proportion and At first supplementary product consumption is the 15-18% of recessed native total weight.
Preferably, the fire retardant is magnesium hydroxide, and the curing agent methyl ethyl ketone peroxide and cobalt octoate liquid are according to weight Component ratio is that 2:1 is matched, and the carbon forming agent is cornstarch.
Preferably, second auxiliary material matches for fire resistance fibre and epoxy vinyl ester resin according to 1:5, and second Supplementary product consumption is the 13-15% of recessed native total weight.
Preferably, the fire resistance fibre is decabromodiphenylethane fire-retardant high-strength polyvinyl, and the epoxy vinyl ester resin is Flame retardant type epoxy vinyl ester resin.
Compared with prior art, the beneficial effects of the present invention are: the present invention can obtain recessed soil using the use of recessed soil Viscosity, while the flame retardant property of recessed soil being effectively utilized, makes full use of the anti-flammability of recessed soil, at the same cooperate other first The addition of auxiliary material and the second auxiliary material further improves flame retardant property, while can obtain good bond properties, easily facilitates It uses.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this Invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not For limiting the present invention.
Embodiment 1
A kind of preparation method of nano concave soil base inorganic flame-retarded agent, the preparation method tool of the nano concave soil base inorganic flame-retarded agent Steps are as follows for body:
S1: the selection of recessed soil selects recessed soil of the purity higher than 98% to be used as recessed soil matrix, is ground, grinds to recessed soil Sieving processing is carried out after mill, the mesh number of recessed soil powder in 2000-3000 mesh, place spare by the recessed native powder of sieving;
S2: recessed soil is stirred, and according to composition by weight ratio is after 1:5 mixing match in blender by recessed native powder and water In be mixed, at 1200 revs/min, the time of mixing controlled at 30 minutes blender revolving speed;
The mixing of S3: the first auxiliary material is added, and continues to be mixed 10 minutes after auxiliary material is added, and blender revolving speed is 600 Rev/min, and the mixing after auxiliary material addition uses the mixing of heating type, temperature when heating is mixed is 80 ℃;
S4: standing, and the material after heating stirring is taken out placement and carries out standing placement in a reservoir, time of repose is at least 3 hours;
S5: the solution upper clear supernate after standing is filtered removal, bottom precipitation is taken out, in drying equipment by filtration treatment Middle carry out drying and processing, drying temperature are controlled at 150 DEG C, and drying time was at 30 minutes;
S6: the material taking-up after drying is carried out secondary milled processed by secondary milled processed in milling apparatus, secondary to grind Treated that powder mesh number takes out after 2000 mesh, grinding is spare for mill;
The mixing of S7: the second auxiliary material is added, and Hybrid Heating stirs after the second auxiliary material is added, the temperature of heating at 110 DEG C, Cooling processing is carried out after being mixed evenly, and is cooled to the laggard luggage bag of room temperature and is sealed spare, the completion inorganic resistance of nano concave earth base Fire the process of agent.
It according to composition by weight ratio is that 1:1:1 is matched that first auxiliary material, which is fire retardant, curing agent and carbon forming agent, described First supplementary product consumption is the 15% of recessed native total weight.The fire retardant be magnesium hydroxide, the curing agent methyl ethyl ketone peroxide with Cobalt octoate liquid is that 2:1 is matched according to composition by weight ratio, and the carbon forming agent is cornstarch.Second auxiliary material is fire-retardant fibre Dimension and epoxy vinyl ester resin are matched according to 1:5, and the second supplementary product consumption is the 13% of recessed native total weight.It is described fire-retardant Fiber is decabromodiphenylethane fire-retardant high-strength polyvinyl, and the epoxy vinyl ester resin is flame retardant type epoxy vinyl ester resin.
Embodiment 2
A kind of preparation method of nano concave soil base inorganic flame-retarded agent, the preparation method tool of the nano concave soil base inorganic flame-retarded agent Steps are as follows for body:
S1: the selection of recessed soil selects recessed soil of the purity higher than 98% to be used as recessed soil matrix, is ground, grinds to recessed soil Sieving processing is carried out after mill, the mesh number of recessed soil powder in 2500 mesh, place spare by the recessed native powder of sieving;
S2: recessed soil is stirred, and according to composition by weight ratio is after 1:5 mixing match in blender by recessed native powder and water In be mixed, at 1400 revs/min, the time of mixing controlled at 40 minutes blender revolving speed;
The mixing of S3: the first auxiliary material is added, and continues to be mixed 13 minutes after auxiliary material is added, and blender revolving speed is 700 Rev/min, and the mixing after auxiliary material addition uses the mixing of heating type, temperature when heating is mixed is 85 ℃;
S4: standing, and the material after heating stirring is taken out placement and carries out standing placement in a reservoir, time of repose is at least 4 hours;
S5: the solution upper clear supernate after standing is filtered removal, bottom precipitation is taken out, in drying equipment by filtration treatment Middle carry out drying and processing, drying temperature are controlled at 170 DEG C, and drying time was at 35 minutes;
S6: the material taking-up after drying is carried out secondary milled processed by secondary milled processed in milling apparatus, secondary to grind Treated that powder mesh number takes out after 2300 mesh, grinding is spare for mill;
The mixing of S7: the second auxiliary material is added, and Hybrid Heating stirs after the second auxiliary material is added, the temperature of heating at 120 DEG C, Cooling processing is carried out after being mixed evenly, and is cooled to the laggard luggage bag of room temperature and is sealed spare, the completion inorganic resistance of nano concave earth base Fire the process of agent.
It according to composition by weight ratio is that 1:1:1 is matched that first auxiliary material, which is fire retardant, curing agent and carbon forming agent, described First supplementary product consumption is the 16% of recessed native total weight.The fire retardant be magnesium hydroxide, the curing agent methyl ethyl ketone peroxide with Cobalt octoate liquid is that 2:1 is matched according to composition by weight ratio, and the carbon forming agent is cornstarch.Second auxiliary material is fire-retardant fibre Dimension and epoxy vinyl ester resin are matched according to 1:5, and the second supplementary product consumption is the 14% of recessed native total weight.It is described fire-retardant Fiber is decabromodiphenylethane fire-retardant high-strength polyvinyl, and the epoxy vinyl ester resin is flame retardant type epoxy vinyl ester resin.
Embodiment 3
A kind of preparation method of nano concave soil base inorganic flame-retarded agent, the preparation method tool of the nano concave soil base inorganic flame-retarded agent Steps are as follows for body:
S1: the selection of recessed soil selects recessed soil of the purity higher than 98% to be used as recessed soil matrix, is ground, grinds to recessed soil Sieving processing is carried out after mill, the mesh number of recessed soil powder in 3000 mesh, place spare by the recessed native powder of sieving;
S2: recessed soil is stirred, and according to composition by weight ratio is after 1:5 mixing match in blender by recessed native powder and water In be mixed, at 1500 revs/min, the time of mixing controlled at 50 minutes blender revolving speed;
The mixing of S3: the first auxiliary material is added, and continues to be mixed 15 minutes after auxiliary material is added, and blender revolving speed is 800 Rev/min, and the mixing after auxiliary material addition uses the mixing of heating type, temperature when heating is mixed is 95 ℃;
S4: standing, and the material after heating stirring is taken out placement and carries out standing placement in a reservoir, time of repose is at least 5 hours;
S5: the solution upper clear supernate after standing is filtered removal, bottom precipitation is taken out, in drying equipment by filtration treatment Middle carry out drying and processing, drying temperature are controlled at 180 DEG C, and drying time was at 40 minutes;
S6: the material taking-up after drying is carried out secondary milled processed by secondary milled processed in milling apparatus, secondary to grind Treated that powder mesh number takes out after 2500 mesh, grinding is spare for mill;
The mixing of S7: the second auxiliary material is added, and Hybrid Heating stirs after the second auxiliary material is added, the temperature of heating at 130 DEG C, Cooling processing is carried out after being mixed evenly, and is cooled to the laggard luggage bag of room temperature and is sealed spare, the completion inorganic resistance of nano concave earth base Fire the process of agent.
It according to composition by weight ratio is that 1:1:1 is matched that first auxiliary material, which is fire retardant, curing agent and carbon forming agent, described First supplementary product consumption is the 18% of recessed native total weight.The fire retardant be magnesium hydroxide, the curing agent methyl ethyl ketone peroxide with Cobalt octoate liquid is that 2:1 is matched according to composition by weight ratio, and the carbon forming agent is cornstarch.Second auxiliary material is fire-retardant fibre Dimension and epoxy vinyl ester resin are matched according to 1:5, and the second supplementary product consumption is the 15% of recessed native total weight.It is described fire-retardant Fiber is decabromodiphenylethane fire-retardant high-strength polyvinyl, and the epoxy vinyl ester resin is flame retardant type epoxy vinyl ester resin.
The present invention can obtain the viscosity of recessed soil using the use of recessed soil, while the flame retardant property of recessed soil being obtained effectively It utilizes, makes full use of the anti-flammability of recessed soil, while the addition of other first auxiliary materials and the second auxiliary material being cooperated further to improve resistance Performance is fired, while good bond properties can be obtained, easily facilitates use.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (5)

1. a kind of preparation method of nano concave soil base inorganic flame-retarded agent, it is characterised in that: the nano concave soil base inorganic flame-retarded agent Specific step is as follows for preparation method:
S1: the selection of recessed soil is selected recessed soil of the purity higher than 98% to be used as recessed soil matrix, is ground to recessed soil, after grinding Sieving processing is carried out, the mesh number of recessed soil powder in 2000-3000 mesh, place spare by the recessed native powder of sieving;
S2: recessed soil is stirred, by recessed native powder and water according to composition by weight ratio be after 1:5 mixing match in blender into Row is mixed, and at 1200-1500 revs/min, the time of mixing controlled at 30-50 minutes blender revolving speed;
The mixing of S3: the first auxiliary material is added, and first auxiliary material is that fire retardant, curing agent and carbon forming agent are according to composition by weight ratio 1:1:1 is matched, and continues to be mixed 10-15 minutes after auxiliary material is added, and blender revolving speed is 600-800 revs/min, and Mixing after auxiliary material addition uses the mixing of heating type, and temperature when heating is mixed is at 80-95 DEG C;
S4: standing, and the material after heating stirring is taken out placement and carries out standing placement in a reservoir, time of repose is at least 3-5 Hour;
S5: filtration treatment, by after standing solution upper clear supernate filter removal, take out bottom precipitation, in drying equipment into Row drying and processing, drying temperature are controlled at 150-180 DEG C, and drying time was at 30-40 minutes;
S6: the material after drying is taken out and carries out secondary milled processed in milling apparatus by secondary milled processed, at secondary grinding Powder mesh number after reason is taken out spare after 2000-2500 mesh, grinding;
The mixing of S7: the second auxiliary material is added, and second auxiliary material is that fire resistance fibre and epoxy vinyl ester resin are matched according to 1:5 It forms, Hybrid Heating stirs after the second auxiliary material is added, and the temperature of heating is dropped after being mixed evenly at 110-130 DEG C Temperature processing, it is spare to be cooled to room temperature laggard luggage bag sealing, completes the process of nano concave soil base inorganic flame-retarded agent.
2. a kind of preparation method of nano concave soil base inorganic flame-retarded agent according to claim 1, it is characterised in that: described One supplementary product consumption is the 15-18% of recessed native total weight.
3. a kind of preparation method of nano concave soil base inorganic flame-retarded agent according to claim 2, it is characterised in that: the resistance Combustion agent is magnesium hydroxide, and the curing agent methyl ethyl ketone peroxide is that 2:1 is matched according to composition by weight ratio with cobalt octoate liquid, institute Stating carbon forming agent is cornstarch.
4. a kind of preparation method of nano concave soil base inorganic flame-retarded agent according to claim 1, it is characterised in that: described Two supplementary product consumptions are the 13-15% of recessed native total weight.
5. a kind of preparation method of nano concave soil base inorganic flame-retarded agent according to claim 4, it is characterised in that: the resistance Combustion fiber is decabromodiphenylethane fire-retardant high-strength polyvinyl, and the epoxy vinyl ester resin is flame retardant type epoxy vinyl ester tree Rouge.
CN201710580377.2A 2017-07-17 2017-07-17 A kind of preparation method of nanometer attapulgite-based inorganic flame retardant Active CN107267162B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102153103A (en) * 2010-12-10 2011-08-17 明光市天骄科技发展有限公司 Preparation method and application of modified attapulgite clay
CN102303960A (en) * 2011-05-20 2012-01-04 上海师范大学 Flame-retarding thermal-insulation composite nano material and preparation method and use thereof
CN103540243A (en) * 2013-10-16 2014-01-29 苏州瑞邦塑胶有限公司 Nano flame-retardant coating

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102153103A (en) * 2010-12-10 2011-08-17 明光市天骄科技发展有限公司 Preparation method and application of modified attapulgite clay
CN102303960A (en) * 2011-05-20 2012-01-04 上海师范大学 Flame-retarding thermal-insulation composite nano material and preparation method and use thereof
CN103540243A (en) * 2013-10-16 2014-01-29 苏州瑞邦塑胶有限公司 Nano flame-retardant coating

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
阻燃、热稳定及耐热矿物分体材料的特性与应用;余丽秀等;《中国粉体技术》;20150430;第21卷(第2期);72-75

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