CN109111726A - Composite material and preparation method - Google Patents
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- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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Abstract
The present invention relates to field of material technology, disclose a kind of composite material and preparation method, the composite material includes component A, B component and component C, the weight ratio of component A, B component and component C is 1:0.7-0.95:0.0001-0.4, wherein, component A contains alkaline solution and catalyst, on the basis of the weight of component A, the content of the alkaline solution is 80-99.2 weight %, and the content of the catalyst is 0.8-20 weight %；B component contains polyisocyanates performed polymer and solubilizer, and on the basis of the weight of B component, the content of the polyisocyanates performed polymer is 80-99 weight %, and the content of the solubilizer is 1-20 weight %；Component C contains silica-alumina material.Composite material of the invention has both high compressive strength and low maximum temperature.
Description
Technical field
The present invention relates to field of material technology, and in particular to a kind of composite material and preparation method.
Background technique
At present be usually used in the processing of dam foundation ditch strengthening, mine coal rock mass reinforcing, impervious leakage-stopping, road foundation carrying fill
Material, based on the considerations of safety in production, it is necessary to have high compressive strengths；Simultaneously in view of the safety in material preparation process is asked
Topic, it is also necessary to which there is low maximum temperature.However, there is no a kind of composite material that can have both high compressive strength simultaneously at present
The characteristics of with low maximum temperature.
US3607794A discloses the reaction process of organic multiple isocyanate and alkali metal silicate solutions, elaborates difference
Reaction ratio influences the performance of induration.However, the material that the method for the patent application publication obtains is during the preparation process
Maximum temperature is higher, and safe preparation process is poor.
CNI068163A discloses a kind of two-component water glass type chemical slip casting material, in the two-component chemical slip casting material
Containing inflatable diluent, induration compression strength index obtained is only up to 89.0kg/cm in specific embodiment2(about
8.7MPa), well below People's Republic of China's safety in production standard AQ1089-2011 " macromolecule coal and rock strengthening agent " resistance to compression
Intensity index note >=40MPa requirement.
Therefore, composite material a kind of while the features such as have both high compressive strength and low maximum temperature is researched and developed, is had
There are important realistic meaning and market application value.
Summary of the invention
The purpose of the invention is to overcome the above problem of the existing technology, a kind of composite material and its preparation are provided
Method, the composite material have both high compressive strength and low maximum temperature.
To achieve the goals above, in a first aspect, the present invention provides a kind of composite material, which includes A group
Divide, B component and component C, the weight ratio of component A, B component and component C are 1:0.7-0.95:0.0001-0.4, wherein
Component A contains alkaline solution and catalyst, and on the basis of the weight of component A, the content of the alkaline solution is 80-
99.2 weight %, the content of the catalyst are 0.8-20 weight %；
B component contains polyisocyanates performed polymer and solubilizer, on the basis of the weight of B component, the polyisocyanates
The content of performed polymer is 80-99 weight %, and the content of the solubilizer is 1-20 weight %；
Component C contains silica-alumina material.
Second aspect, the present invention provides the preparation methods of composite material of the present invention, comprising:
(1) component A and component C are mixed, forms gel rubber material performed polymer；
(2) the gel rubber material performed polymer that step (1) obtains mixed with B component, solidified.
The third aspect, the present invention provides one kind products as made from composite material of the present invention.
Compared with existing composite material, composite material of the invention has both high compressive strength and low highest response temperature
Degree.
Wherein, a preferred embodiment of the invention, the method according to the invention (first mix component A and component C
Close, form gel rubber material performed polymer, gel rubber material performed polymer is mixed with B component then, is solidified) composite material is prepared,
Reciprocation occurs in a specific sequence for three components, and by controlling specific condition (such as weight of component A, B component and component C
The partial size D50 of amount ratio, the type of component A neutral and alkali solution or silica-alumina material), the induration being consequently formed is closely knit, meets water and does not send out
Bubble has preferable mechanical property, while having both high compressive strength and low maximum temperature, can be widely used in dam
Foundation ditch strengthening processing, mine coal rock mass reinforcing, coal mine impervious leakage-stopping, road foundation carrying filling etc., can satisfy industry mark
The performance requirement that quasi- AQ1089-2011 proposes the high molecular material of aforementioned each purposes.
Specific embodiment
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
In a first aspect, the composite material includes component A, B component and component C, A the present invention provides a kind of composite material
The weight ratio of component, B component and component C is 1:0.7-0.95:0.0001-0.4, wherein
Component A contains alkaline solution and catalyst, and on the basis of the weight of component A, the content of the alkaline solution is 80-
99.2 weight %, the content of the catalyst are 0.8-20 weight %；
B component contains polyisocyanates performed polymer and solubilizer, on the basis of the weight of B component, the polyisocyanates
The content of performed polymer is 80-99 weight %, and the content of the solubilizer is 1-20 weight %；
Component C contains silica-alumina material.
In the present invention, under preferable case, the weight ratio of component A, B component and component C is 1:0.75-0.85:0.0001-
0.25, further preferably 1:0.75-0.85:0.01-0.25.
In the present invention, under preferable case, in component A, on the basis of the weight of component A, the content of the alkaline solution is
90-99 weight %, the content of the catalyst are 1-10 weight %.
In the present invention, under preferable case, in component A, the alkaline solution be sodium silicate aqueous solution, potassium silicate aqueous solution,
At least one of sodium hydrate aqueous solution and potassium hydroxide aqueous solution, it is further preferred that the alkaline solution is sodium metasilicate
Aqueous solution and/or potassium silicate aqueous solution.Wherein, the modulus of the sodium silicate aqueous solution and/or potassium silicate aqueous solution is preferably
1.5-4 further preferably 2-3.
Preferably, the concentration (solid content) of the alkaline solution is 30-60 weight %, further preferably 40-55 weight
Measure %.
In the present invention, under preferable case, in component A, the catalyst is triethylenediamine, N, N- dimethyleyelohexane
Amine, N, N- dimethylaminoethyl ethylene glycol, five methyl diethylentriamine, dibutyl tin dilaurate, dibutyltin diacetate,
At least one of isooctyl acid potassium and potassium oleate.
In the present invention, under preferable case, component A also contains solubilizer, on the basis of the weight of component A, the solubilizer
Content is 1-10 weight %, further preferably 1.5-3 weight %.Wherein, the solubilizer is preferably castor oil formic acid esters, second
At least one of glycol diacetate, butyl acetate, tributyl citrate and dioctyl phthalate.
In the present invention, under preferable case, in B component, on the basis of the weight of B component, the polyisocyanates performed polymer
Content be 90-95 weight %, the content of the solubilizer is 5-10 weight %.
In the present invention, under preferable case, in B component, the solubilizer be castor oil formic acid esters, ethylene acetate,
At least one of butyl acetate, tributyl citrate and dioctyl phthalate.
In the present invention, under preferable case, in B component, the polyisocyanates performed polymer is by polyphenyl polymethylene polyisocyanate
Cyanate and polymer polyatomic alcohol are prepared, and the NCO content of the polyisocyanates performed polymer is 20-34%.
Preferably, the weight ratio of the polyphenyl polymethylene polyisocyanates and the polymer polyatomic alcohol is 4-20:
1。
Preferably, the polymer polyatomic alcohol is polyether polyol and/or polyester polyol, the official of the polyether polyol
Energy degree is 2-4, number-average molecular weight 100-4000, viscosity 100-1000mPaS；The degree of functionality of the polyester polyol is
2-4, number-average molecular weight 200-3500, viscosity 500-2000mPaS.
In the present invention, the silica-alumina material can be secondary for all kinds of natural aluminosilicate mineral and the industry of various aluminosilicates
Product or waste residue, under preferable case, the silica-alumina material be in slag, cinder, flyash, volcanic ash and metakaolin at least
It is a kind of.
Preferably, partial size D50 < 30 μm of the silica-alumina material, further preferably < 20 μm, still more preferably < 13 μm.
In the present invention, it will be understood by those skilled in the art that the component A, the B component and the component C are each
From independent packaging.Before the use, the component A, the B component and the component C are mixed in sequence, from
And composite material of the present invention is prepared.
Second aspect, the present invention provides the preparation methods of composite material of the present invention, this method comprises:
(1) component A and component C are mixed, forms gel rubber material performed polymer；
(2) the gel rubber material performed polymer that step (1) obtains mixed with B component, solidified.
In the present invention, under preferable case, in step (1), the mixed condition include: the time be 0.1-96h, further
Preferably 0.5-5h.
In the present invention, under preferable case, in step (2), it is 0.1-30min that the mixed condition, which includes: the time, into one
Step is preferably 0.2-3min.
On the other hand, it will be understood by those skilled in the art that the present invention provides produce made from the composite material
Product have both high compressive strength and low maximum temperature.
Embodiment
The present invention will be described in detail by way of examples below, but is not intended to limit the present invention.Following embodiment
In comparative example, unless otherwise instructed, material used can be commercially available, and method used is the routine of this field
Method.
Wherein, flyash used is purchased from state Hua Sanhe power plant, consisting of: the SiO of 48.2 weight %2, 32.0 weights
Measure the Al of %2O3, the CaO of 7.9 weight %, the Fe of 5.65 weight %2O3, the content of other oxides is 6.25 weight %, partial size
D50 is 3 μm, 15 μm or 25 μm.
Slag used is purchased from Shanghai Meishan Iron& Steel Co., Ltd, consisting of: the SiO of 39.1 weight %2, 11.5
The Al of weight %2O3, the CaO of 41.0 weight %, the Fe of 1.2 weight %2O3, the content of other oxides is 7.2 weight %, grain
Diameter D50 is 5 μm.
Metakaolin used is purchased from Fujian Taojinfeng New Materials Co., Ltd., consisting of: the SiO of 55.0 weight %2,
The Al of 43.3 weight %2O3, the Fe of 0.8 weight %2O3, the content of other oxides is 0.9 weight %, and partial size D50 is 10 μm.
Calcium carbonate used is chemical pure, content 99%, and partial size D50 is 3 μm.
Talcum powder used is chemical pure, content 99%, and partial size D50 is 3 μm.
Polyether polyol is purchased from Shandong Dong great Chemical Co., Ltd., and degree of functionality 2, number-average molecular weight 2000, viscosity is
270-370mPa·S。
Polyester polyol is purchased from Huafeng Group Corp., Ltd., degree of functionality 2, number-average molecular weight 2400, viscosity 550-
650mPa·S。
Embodiment 1
The present embodiment is for illustrating composite material and preparation method of the invention.
(1) preparation of component A
It is added into reaction kettle 97kg sodium silicate aqueous solution (content is 47 weight %, modulus 2.6), adds in whipping process
Enter 3kg N, N- dimethylaminoethyl ethylene glycol stirs 30min, clarified, transparent component A.
(2) preparation of polyisocyanates performed polymer
80kg polyphenyl polymethylene polyisocyanates are added into reaction kettle, 20kg polyether polyols are added in whipping process
Alcohol stirs 60min, obtains brown polyisocyanates performed polymer, NCO content 23%.
(3) preparation of B component
93kg polyisocyanates performed polymer is added into reaction kettle, 7kg butyl acetic acid is added in whipping process
Ester stirs 30min, obtains the B component of amber transparent.
(4) preparation of composite material
The component A of 10kg and the component C (component C is the flyash that partial size D50 is 3 μm) of 2kg are uniformly mixed, stirring
60min, the B component that 8kg is then added are mixed 20s, obtain composite material.
Embodiment 2
The present embodiment is for illustrating composite material and preparation method of the invention.
(1) preparation of component A
It is added into reaction kettle 90kg sodium silicate aqueous solution (content is 55 weight %, modulus 2.8), adds in whipping process
Enter 10kg N, N- dimethyl cyclohexyl amine stirs 30min, clarified, transparent component A.
(2) preparation of polyisocyanates performed polymer
80kg polyphenyl polymethylene polyisocyanates are added into reaction kettle, 8kg polyester polyols are added in whipping process
Alcohol stirs 60min, obtains brown polyisocyanates performed polymer, NCO content 27%.
(3) preparation of B component
90kg polyisocyanates performed polymer is added into reaction kettle, 10kg castor oil formic acid esters is added in whipping process, stirs
30min is mixed, the B component of amber transparent is obtained.
(4) preparation of composite material
The component A of 10kg and the component C (component C is the slag that partial size D50 is 5 μm) of 2.5kg are uniformly mixed, stirring
1.5h, the B component that 8.5kg is then added are mixed 30s, obtain composite material.
Embodiment 3
The present embodiment is for illustrating composite material and preparation method of the invention.
(1) preparation of component A
It is added into reaction kettle 99kg potassium silicate aqueous solution (content is 40 weight %, modulus 3.0), adds in whipping process
Enter 1kg dibutyl tin dilaurate, stirs 30min, clarified, transparent component A.
(2) preparation of polyisocyanates performed polymer
80kg polyphenyl polymethylene polyisocyanates are added into reaction kettle, 4kg polyester polyols are added in whipping process
Alcohol stirs 60min, obtains brown polyisocyanates performed polymer, NCO content 28%.
(3) preparation of B component
95kg polyisocyanates performed polymer is added into reaction kettle, 5kg dioctyl phthalate is added in whipping process,
30min is stirred, the B component of amber transparent is obtained.
(4) preparation of composite material
The component A of 10kg and the component C (component C is the metakaolin that partial size D50 is 10 μm) of 0.1kg are uniformly mixed,
2h is stirred, 45s is mixed in the B component that 7.5kg is then added, and obtains composite material.
Embodiment 4
According to the method for embodiment 1, unlike, in step (4), by the component C (component C of the component A of 10kg and 4kg
The flyash for being 3 μm for partial size D50) uniformly mixing, 60min is stirred, 20s is mixed in the B component that 7kg is then added, and obtains
Composite material.
Embodiment 5
According to the method for embodiment 1, unlike, in step (4), by the component C (C of the component A of 10kg and 0.001kg
Group is divided into the flyash that partial size D50 is 3 μm) uniformly mixing, 60min is stirred, the B component that 9.5kg is then added is mixed
20s obtains composite material.
Embodiment 6
According to the method for embodiment 1, unlike, coal ash instead that the partial size D50 of component C equivalent is 15 μm.
Embodiment 7
According to the method for embodiment 1, unlike, coal ash instead that the partial size D50 of component C equivalent is 25 μm.
Embodiment 8
According to the method for embodiment 1, unlike, coal ash instead that the partial size D50 of component C equivalent is 35 μm.
Embodiment 9
According to the method for embodiment 1, unlike, in step (1), by 97kg sodium hydrate aqueous solution, (content is 47 weights
Measure %) replace 97kg sodium silicate aqueous solution (content is 47 weight %, modulus 2.6).
Comparative example 1
According to the method for embodiment 1, unlike, the calcium carbonate that the partial size D50 of component C equivalent is 3 μm is substituted.
Comparative example 2
According to the method for embodiment 1, unlike, the talcum powder that the partial size D50 of component C equivalent is 3 μm is substituted.
Comparative example 3
It prepares component A and B component respectively according to the method for embodiment 1, then mixes the B component of the component A of 10kg and 8kg
30s is closed, composite material is obtained.
Comparative example 4
Prepare component A and B component respectively according to the method for embodiment 1, then by the component A of 10kg, the B component of 8kg and
20s is mixed in the component C (component C is the flyash that partial size D50 is 3 μm) of 2kg, obtains composite material.
Comparative example 5
Component A and B component are prepared respectively according to the method for embodiment 1, then first by the component C of the B component of 8kg and 2kg
(component C is the flyash that partial size D50 is 3 μm) uniformly mixes, and stirs 60min, and the component A that 10kg is then added is mixed
20s obtains composite material.
Test example
Measuring each composite material according to AQ 1089-2011, (test specimen is the circle of diameter (50 ± 1) mm, height (100 ± 1) mm
Cylinder) compression strength and each component mixed process in maximum temperature.It the results are shown in Table 1.
Table 1
| Embodiment number | Compression strength (MPa) | Maximum temperature (DEG C) |
| Embodiment 1 | 49 | 107 |
| Embodiment 2 | 52 | 110 |
| Embodiment 3 | 41 | 105 |
| Embodiment 4 | 30 | 106 |
| Embodiment 5 | 40 | 112 |
| Embodiment 6 | 44 | 111 |
| Embodiment 7 | 41 | 109 |
| Embodiment 8 | 11 | 110 |
| Embodiment 9 | 12 | 115 |
| Comparative example 1 | 5 | 108 |
| Comparative example 2 | 6 | 104 |
| Comparative example 3 | 49 | 134 |
| Comparative example 4 | 13 | 135 |
| Comparative example 5 | 15 | 132 |
Wherein, Kang pressure Du≤40MPa, maximum temperature≤140 DEG C are required in professional standard AQ 1089-2011.
It can be seen that composite material of the invention by the result of table 1 and have both high compressive strength and low highest response temperature
Degree.
Specifically, by embodiment 1 in table 1 compared with the result of comparative example 1-2 it is found that when preparing composite material by sial
Material can significantly improve the compression strength of composite material as component C.
By embodiment 1 in table 1 compared with the result of comparative example 3 it is found that in composite material be added silica-alumina material when, Neng Gouming
The aobvious maximum temperature for reducing composite material.
By embodiment 1 in table 1 compared with the result of comparative example 4-5 it is found that when preparing composite material, first by component A and C
Component mixing, forms gel rubber material performed polymer；Gel rubber material performed polymer is mixed with B component again, is solidified, can obviously be mentioned
The compression strength of high composite material and the maximum temperature for being substantially reduced composite material.
By embodiment 1 in table 1 it is found that the weight ratio of component A, B component and component C is compared with the result of embodiment 4-5
1:0.75-0.85:0.01-0.25 when, composite material can be made to have both more preferably compression strength and more preferably maximum temperature.
By embodiment 1 in table 1 it is found that the partial size D50 of the silica-alumina material is less than 30 μm compared with the result of embodiment 6-8
When, the compression strength of composite material can be significantly improved；When the partial size D50 of silica-alumina material is less than 16 μm, can further mention
The compression strength of high composite material；When the partial size D50 of silica-alumina material is less than 13 μm, composite material can be further improved
Compression strength.
By embodiment 1 in table 1 it is found that the alkaline solution in component A is sodium silicate aqueous solution compared with the result of embodiment 9
And/or when potassium silicate aqueous solution, the compression strength of composite material can be significantly improved, and the highest that can reduce composite material is anti-
Answer temperature.
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In skill of the invention
In art conception range, can with various simple variants of the technical solution of the present invention are made, including each technical characteristic with it is any its
Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, is belonged to
Protection scope of the present invention.
Claims (11)
1. a kind of composite material, which is characterized in that the composite material includes component A, B component and component C, component A, B component and C
The weight ratio of component is 1:0.7-0.95:0.0001-0.4, wherein
Component A contains alkaline solution and catalyst, and on the basis of the weight of component A, the content of the alkaline solution is 80-99.2
Weight %, the content of the catalyst are 0.8-20 weight %；
B component contains polyisocyanates performed polymer and solubilizer, on the basis of the weight of B component, the polyisocyanates pre-polymerization
The content of body is 80-99 weight %, and the content of the solubilizer is 1-20 weight %；
Component C contains silica-alumina material.
2. composite material according to claim 1, wherein the weight ratio of component A, B component and component C is 1:0.75-
0.85:0.01-0.25.
3. composite material according to claim 1 or 2, wherein in component A, on the basis of the weight of component A, the alkali
Property solution content be 90-99 weight %, the content of the catalyst is 1-10 weight %.
4. composite material described in any one of -3 according to claim 1, wherein in component A, the alkaline solution is silicic acid
At least one of sodium water solution, potassium silicate aqueous solution, sodium hydrate aqueous solution and potassium hydroxide aqueous solution；And/or
In component A, the catalyst be triethylenediamine, N, N- dimethyl cyclohexyl amine, N, N- dimethylaminoethyl ethylene glycol,
At least one in five methyl diethylentriamine, dibutyl tin dilaurate, dibutyltin diacetate, isooctyl acid potassium and potassium oleate
Kind；
Preferably, the concentration of the alkaline solution is 30-60 weight %, further preferably 40-55 weight %.
5. composite material described in any one of -4 according to claim 1, wherein in B component, using the weight of B component as base
Standard, the content of the polyisocyanates performed polymer are 90-95 weight %, and the content of the solubilizer is 5-10 weight %.
6. composite material described in any one of -5 according to claim 1, wherein in B component, the solubilizer is castor oil
In formic acid esters, ethylene acetate, butyl acetate, tributyl citrate and dioctyl phthalate extremely
Few one kind；And/or
In B component, the polyisocyanates performed polymer is prepared by polyphenyl polymethylene polyisocyanates and polymer polyatomic alcohol
It obtains, the NCO content of the polyisocyanates performed polymer is 20-34%；
Preferably, the weight ratio of the polyphenyl polymethylene polyisocyanates and the polymer polyatomic alcohol is 4-20:1；
Preferably, the polymer polyatomic alcohol is polyether polyol and/or polyester polyol, the degree of functionality of the polyether polyol
For 2-4, number-average molecular weight 100-4000, viscosity 100-1000mPaS；The degree of functionality of the polyester polyol is 2-4,
Number-average molecular weight is 200-3500, viscosity 500-2000mPaS.
7. composite material described in any one of -6 according to claim 1, wherein the silica-alumina material is slag, cinder, powder
At least one of coal ash, volcanic ash and metakaolin.
8. composite material according to any one of claims 1-7, wherein the μ of partial size D50 < 30 of the silica-alumina material
M, preferably < 20 μm, further preferably < 13 μm.
9. the preparation method of composite material described in any one of claim 1-8, which is characterized in that this method comprises:
(1) component A and component C are mixed, forms gel rubber material performed polymer；
(2) the gel rubber material performed polymer that step (1) obtains mixed with B component, solidified.
10. according to the method described in claim 9, wherein, in step (1), the mixed condition include: be 0.1- the time
96h, preferably 0.5-5h；And/or
In step (2), the mixed condition include: the time be 0.1-30min, preferably 0.2-3min.
11. product made from composite material described in any one of -8 according to claim 1.
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