CN107189338A - A kind of combined binder used for refractory material and preparation method thereof - Google Patents
A kind of combined binder used for refractory material and preparation method thereof Download PDFInfo
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- CN107189338A CN107189338A CN201710445207.3A CN201710445207A CN107189338A CN 107189338 A CN107189338 A CN 107189338A CN 201710445207 A CN201710445207 A CN 201710445207A CN 107189338 A CN107189338 A CN 107189338A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/175—Amines; Quaternary ammonium compounds containing COOH-groups; Esters or salts thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/20—Carboxylic acid amides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/41—Compounds containing sulfur bound to oxygen
- C08K5/42—Sulfonic acids; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/006—Additives being defined by their surface area
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention provides a kind of combined binder used for refractory material and preparation method thereof, the combined binder used for refractory material is made up of the raw material of following parts by weight：70~80 parts of phenolic resin, 50~60 parts of absolute ethyl alcohol, 0.5~2 part of modified white carbon black, 0.5~1.5 part of formaldehyde catching agent, the formaldehyde catching agent is the compound containing primary amine group.The present invention is modified using modified white carbon black and formaldehyde catching agent to traditional phenolic resin binder, improves heat resistance, the caking property of bonding agent；The content of free phenol is reduced, obtained combined binder used for refractory material more environmental protection is safe；Cost of material is low, and preparation technology is simple, easy control of reaction conditions, it is easy to prepared by large-scale production.
Description
Technical field
The present invention relates to technical field of refractory materials, more particularly to a kind of high-adhesion, environmental protection it is used for refractory material
Combined binder and preparation method thereof.
Background technology
" bottleneck " of the refractories industry development of restriction China, economy and market development shape are increasingly becoming in resource, environment
In the case that gesture changes, the development of refractories industry is faced with multiple test and challenge.In recent years, due to fire resisting
Product high yield rate, production cost is low and function admirable, thus have developed rapidly, and new varieties emerge in an endless stream, and obtain significant society
Can economic benefit.However, for many materials using environmental pollution in traditional refractory material of refractory product, such as bonding agent
Use phenolic resin and pitch, phenolic resin has the advantages that adhesion strength is big, heat-resisting as binder for fire-resistant materials more, but its
Not only cost is high for the refractory material prepared, also contain free phenol, dissociate the noxious materials such as aldehyde, is unfavorable for environmental protection；In addition, drip
Blue or green and its flue gas has excitant to mucocutaneous, there is light toxic action and carcinogenesis.Because formaldehyde is studied by international cancer
Mechanism (IARC) regards as carcinogenic substance, and low content of free formaldehyde content has also turned into a requirement.However, specific resin should be kept
Property and take into account low free-phenol and low content of free formaldehyde is very difficult.
Disclosed in Chinese patent literature a kind of " refractory material ", its notification number is CN104844238A, the invention is provided
Lignin-sugar composite can partly substitute phenolic resin as the adhesive of refractory material, its bonding effect is good, especially
Suitable for fields such as non-burning refractory brick, iron runner materials.But the adhesive property of lignin-sugar composite is substantially reduced, for fire resisting
The preparation of material is unfavorable for good yields, and the function of the phenolic resin of refractory material can not be substituted completely, it is impossible to from
Fundamentally solve pollution problem of the refractory material to environment.Therefore, new technology, new raw material and regenerated resources how to be increased in fire resisting
Application in design of material and manufacturing process, exploitation energy-conservation and environmental-protecting process, the combined binder used for refractory material of new varieties,
The material of environmental pollution is reduced or substitutes, it is this area skill to promote refractories industry environmental protection and the raising of occupational health level
Art personnel's urgent problem to be solved.
The content of the invention
There is provided a kind of high bonding in order to overcome the problem of existing refractory binder has environmental pollution by the present invention
Property, high-fire resistance, the combined binder used for refractory material of environmental protection.
It is a further object to provide a kind of preparation method of the simple combined binder used for refractory material of technique.
To achieve these goals, the present invention uses following technical scheme：
A kind of combined binder used for refractory material, the combined binder used for refractory material is made up of the raw material of following parts by weight：
70~80 parts of phenolic resin, 50~60 parts of absolute ethyl alcohol, 0.5~2 part of modified white carbon black, 0.5~1.5 part of formaldehyde catching agent, institute
Formaldehyde catching agent is stated for the compound containing primary amine group.
The modified white carbon black that the present invention is used is porous material, and its composition can use SiO2·nH2O represents, can be uniform and good
It is scattered in phenolic resin as matrix resin well, so as to improve the carbon yield and inoxidizability of phenolic resin, combines phenolic resin
The performance of agent is improved；Modified white carbon is spherical in shape, uniformly can well disperse in phenolic resin as matrix resin, disperses effect
It is really good, Si atoms are introduced on phenolic resin so that silicon dioxide molecules are connected in the form of chemical bond with phenolic resin
Connect, rather than be simply blended with phenolic resin.In addition, the price of white carbon is lower than other nano silicons, life is reduced
Cost is produced, beneficial to industrialized production.
Preferably, the formaldehyde catching agent has following formula：R-NH2, wherein, R is selected from-OH ,-CH2-CH2-SO3H ,-CH2
And-CH (COOH) (CH (COOH)2CH2CONH2) in one or more.
The present invention also uses the compound for containing primary amine group as formaldehyde catching agent, and its reaction principle is：Acid condition
Under, nucleophilic can occur under the conditions of 45~60 DEG C for the carbonyl for the aldehyde that dissociates in the primary amine group and phenolic resin in formaldehyde catching agent
Addition reaction generates RNHCH2OH, the structural stability is very poor, can generate RNH=CH with rapid dehydration2, and occur from each other
Condensation reaction, forms polymeric crosslinker.On the one hand the reaction can dissociate in reduction system the content of aldehyde, on the other hand can be with
The network-like polymeric crosslinker of generation, can improve its heat resistance and caking property to phenolic resin modified toughness reinforcing.-CH
(COOH)(CH2CH2CONH2) be amino acid formula, the present invention in amino acid be selected from isoleucine, glutamine, the third ammonia
Acid, valine, lysine, arginine, histidine, methionine, threonine, glycine, serine, cysteine, and its salt.
Preferably, the granularity of the modified white carbon black is 7~40nm, specific surface area is 150~400m2/g。
Preferably, the preparation method of the modified white carbon black is：White carbon is first activated 5 under the conditions of 450~600 DEG C
~10h, adds absolute ethyl alcohol, is configured to 4~10wt% silica sol；Polysorbas20 is added dropwise under the conditions of 50~60 DEG C again to arrive
In silica sol, 15~30min of stirring reaction, 5~30min of sonic oscillation obtain modified white carbon black.
The modifying agent selected by process that the present invention is modified to white carbon is polysorbas20, due to poly- sorb in polysorbas20
There are the more polyoxyethylene groups of hydrophilic radical one in ester molecule, therefore hydrophily is strong, is a kind of nonionic surface active agent, can
To modify white carbon so that white carbon epoxide epoxy group group has higher activity, easily occurs open loop addition, on phenolic resin
Introduce Si atoms so that nano silicon molecule is attached in the form of chemical bond with phenolic resin, rather than simply
And phenol
Urea formaldehyde is blended, so that the content of free phenol in phenolic resin is reduced, safer, environmental protection.
A kind of preparation method of combined binder used for refractory material, comprises the following steps：
(1) raw material is weighed respectively according to said ratio, absolute ethyl alcohol, formulated phenolic resin solution are added in phenolic resin；
(2) modified white carbon black is added in the phenol resin solution in step (1), 3~6h is stirred under the conditions of 55~60 DEG C,
Phenol-formaldehyde resin modified mixed liquor is made；
(3) formaldehyde catching agent is added to the phenol-formaldehyde resin modified mixed liquor obtained in step (2), it is anti-under the conditions of 45~60 DEG C
Answer and combined binder used for refractory material is obtained after 15~60min, cooling.
Preferably, the pH of phenol-formaldehyde resin modified mixed liquor described in step (3) is controlled 2~5.
Under acid condition, nucleophilic addition occurs for the primary amine group in the carbonyl and formaldehyde catching agent of aldehyde that dissociate, then
Dehydration, polycondensation generation condensation polymer, when pH value control is 2~5, the degree of polymerization is optimal, obtained combined binder used for refractory material
Refractoriness and cementability it is optimal.
The present invention has the advantages that：
(1) traditional phenolic resin binder is modified using modified white carbon black and formaldehyde catching agent, improves bonding agent
Heat resistance, caking property；
(2) content of free phenol is reduced, obtained combined binder used for refractory material more environmental protection is safe；
(3) cost of material is low, and preparation technology is simple, easy control of reaction conditions, it is easy to prepared by large-scale production.
Embodiment
Below by specific embodiment, technical scheme is described in further detail.
In the present invention, if not refering in particular to, all devices and raw material are commercially available or the industry is conventional, following
Method in embodiment, is this area conventional method unless otherwise instructed.
Embodiment 1
(1) modified white carbon black is prepared standby：White carbon is first activated into 5h under the conditions of 450 DEG C, absolute ethyl alcohol is added, is configured to
4wt% silica sol；Polysorbas20 is added dropwise under the conditions of 50 DEG C again into silica sol, stirring reaction 15min, ultrasound is shaken
5min is swung, modified white carbon black is obtained；
Phenolic resin 70g, absolute ethyl alcohol 50g, modified white carbon black (particle mean size 7nm, specific surface area 150m are weighed respectively2/g)
0.5g, 0.5g H2N-CH2-CH2-SO3H；Absolute ethyl alcohol, formulated phenolic resin solution are added in phenolic resin；
(2) modified white carbon black is added in the phenol resin solution in step (1), 3h is stirred under the conditions of 55 DEG C, be made and change
Property phenolic resin mixed liquor；
(3) by H2N-CH2-CH2-SO3H is added to the phenol-formaldehyde resin modified mixed liquor (pH=2) obtained in step (2), in 45 DEG C
Under the conditions of react combined binder used for refractory material obtained after 60min, cooling.
Embodiment 2
(1) modified white carbon black is prepared standby：White carbon is first activated into 10h under the conditions of 600 DEG C, absolute ethyl alcohol is added, is configured to
10wt% silica sol；Polysorbas20 is added dropwise under the conditions of 60 DEG C again into silica sol, stirring reaction 30min, ultrasound
30min is vibrated, modified white carbon black is obtained；
Phenolic resin 80g, absolute ethyl alcohol 60g, modified white carbon black (particle mean size 40nm, specific surface area 400m are weighed respectively2/g)
2g, 0.5g H2N-CH(COOH)(CH2CH2CONH2), 1g NH2OH；Absolute ethyl alcohol is added in phenolic resin, phenolic aldehyde is prepared
Resin solution；
(2) modified white carbon black is added in the phenol resin solution in step (1), 6h is stirred under the conditions of 60 DEG C, be made and change
Property phenolic resin mixed liquor；
(3) by H2N-CH(COOH)(CH2CH2CONH2) and NH2OH is added separately to the phenol-formaldehyde resin modified obtained in step (2)
Mixed liquor (pH=5), reacts under the conditions of 60 DEG C and combined binder used for refractory material is obtained after 15min, cooling.
Embodiment 3
(1) modified white carbon black is prepared standby：White carbon is first activated into 8h under the conditions of 550 DEG C, absolute ethyl alcohol is added, is configured to
7wt% silica sol；Polysorbas20 is added dropwise under the conditions of 55 DEG C again into silica sol, stirring reaction 20min, ultrasound is shaken
15min is swung, modified white carbon black is obtained；
Phenolic resin 75g, absolute ethyl alcohol 55g, modified white carbon black (particle mean size 20nm, specific surface area 200m are weighed respectively2/g)
1g, 0.3g NH2OH and 0.7g H2N-CH2(COOH)；Absolute ethyl alcohol, formulated phenolic resin solution are added in phenolic resin；
(2) modified white carbon black is added in the phenol resin solution in step (1), 4h is stirred under the conditions of 58 DEG C, be made and change
Property phenolic resin mixed liquor；
(3) by NH2OH and H2N-CH2(COOH) it is added separately to the phenol-formaldehyde resin modified mixed liquor (pH=obtained in step (2)
2), reacted under the conditions of 50 DEG C and combined binder used for refractory material is obtained after 35min, cooling.
Comparative example
Comparative example uses commercial phenolic resin.
The physical and chemical index of the commercial phenolic resin of combined binder used for refractory material and comparative example to embodiment 1-3 is carried out
Detection, as a result as shown in table 1.
The physical and chemical index result of table 1.
| Physical and chemical index | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example |
| Solid content, wt% | 87 | 88 | 90 | 80 |
| Free phenol, wt% | 2 | 8 | 5 | 15 |
| Free aldehyde, wt% | 0.3 | 0.2 | 0.5 | 5 |
| Heat resistance, DEG C | 1345 | 1350 | 1380 | 1200 |
As can be seen from Table 1, the formaldehyde catching agent by modified white carbon black and containing primary amine group is to traditional phenolic resin knot
Mixture is modified, obtained combined binder used for refractory material relative to commercial phenolic resin caking property and heat resistance more
Height, and greatly reduce the content of free phenol, aldehyde, more environmental protection.
The present invention is modified using modified white carbon black and formaldehyde catching agent to traditional phenolic resin binder, is improved
Heat resistance, the caking property of bonding agent；The content of free phenol, aldehyde is reduced, obtained combined binder used for refractory material is more green
Colour circle is protected, safe；Cost of material is low, and preparation technology is simple, easy control of reaction conditions, it is easy to prepared by large-scale production.
Claims (6)
1. a kind of combined binder used for refractory material, it is characterised in that the combined binder used for refractory material is by following weight
The raw material of part is made：70~80 parts of phenolic resin, 50~60 parts of absolute ethyl alcohol, 0.5~2 part of modified white carbon black, formaldehyde catching agent
0.5~1.5 part, the formaldehyde catching agent is the compound containing primary amine group.
2. a kind of combined binder used for refractory material according to claim 1, it is characterised in that the formaldehyde catching agent tool
There is following formula：R-NH2, wherein, R is selected from-OH ,-CH2-CH2-SO3H ,-CH2And-CH (COOH) (CH (COOH)2CH2CONH2) in
It is one or more of.
3. a kind of combined binder used for refractory material according to claim 1 or 2, it is characterised in that the modified hard charcoal
Black granularity is 7~40nm, and specific surface area is 150~400m2/g。
4. a kind of combined binder used for refractory material according to claim 1, it is characterised in that the modified white carbon black
Preparation method is：White carbon is first activated into 5~10h under the conditions of 450~600 DEG C, absolute ethyl alcohol is added, it is configured to 4~
10wt% silica sol；Polysorbas20 is added dropwise under the conditions of 50~60 DEG C again into silica sol, stirring reaction 15~
30min, 5~30min of sonic oscillation, obtains modified white carbon black.
5. the preparation method of a kind of combined binder used for refractory material as described in requiring 1, it is characterised in that including following step
Suddenly：
(1) raw material is weighed respectively according to said ratio, absolute ethyl alcohol, formulated phenolic resin solution are added in phenolic resin；
(2) modified white carbon black is added in the phenol resin solution in step (1), 3~6h is stirred under the conditions of 55~60 DEG C,
Phenol-formaldehyde resin modified mixed liquor is made；
(3) formaldehyde catching agent is added to the phenol-formaldehyde resin modified mixed liquor obtained in step (2), it is anti-under the conditions of 45~60 DEG C
Answer and combined binder used for refractory material is obtained after 15~60min, cooling.
6. the preparation method of combined binder used for refractory material according to claim 5, it is characterised in that in step (3)
The pH of the phenol-formaldehyde resin modified mixed liquor is controlled 2~5.
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| CN201710445207.3A CN107189338A (en) | 2017-06-13 | 2017-06-13 | A kind of combined binder used for refractory material and preparation method thereof |
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| CN201710445207.3A CN107189338A (en) | 2017-06-13 | 2017-06-13 | A kind of combined binder used for refractory material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108059926A (en) * | 2017-11-14 | 2018-05-22 | 浙江元集新材料科技股份有限公司 | A kind of preparation method of the special high heat conduction bonding sheet of aluminum-based copper-clad plate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942286A (en) * | 2010-09-21 | 2011-01-12 | 武汉科技大学 | Composite bonding agent for sliding plate refractory material and preparation method thereof |
| CN103221443A (en) * | 2010-08-27 | 2013-07-24 | 圣戈班伊索福公司 | Phenolic resin, method for preparing same, sizing composition for mineral fibers and resulting product |
| CN103282395A (en) * | 2010-10-01 | 2013-09-04 | 迪纳化学公司 | Low free formaldehyde phenolic resins for abrasive products |
-
2017
- 2017-06-13 CN CN201710445207.3A patent/CN107189338A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103221443A (en) * | 2010-08-27 | 2013-07-24 | 圣戈班伊索福公司 | Phenolic resin, method for preparing same, sizing composition for mineral fibers and resulting product |
| CN101942286A (en) * | 2010-09-21 | 2011-01-12 | 武汉科技大学 | Composite bonding agent for sliding plate refractory material and preparation method thereof |
| CN103282395A (en) * | 2010-10-01 | 2013-09-04 | 迪纳化学公司 | Low free formaldehyde phenolic resins for abrasive products |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108059926A (en) * | 2017-11-14 | 2018-05-22 | 浙江元集新材料科技股份有限公司 | A kind of preparation method of the special high heat conduction bonding sheet of aluminum-based copper-clad plate |
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Application publication date: 20170922 |