CN112919845A - Grinding aid containing waste liquid generated by caprolactam rearrangement reaction and application thereof - Google Patents
Grinding aid containing waste liquid generated by caprolactam rearrangement reaction and application thereof Download PDFInfo
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- CN112919845A CN112919845A CN202110230119.8A CN202110230119A CN112919845A CN 112919845 A CN112919845 A CN 112919845A CN 202110230119 A CN202110230119 A CN 202110230119A CN 112919845 A CN112919845 A CN 112919845A
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- grinding aid
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
- C04B20/023—Chemical treatment
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/52—Grinding aids; Additives added during grinding
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
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- General Chemical & Material Sciences (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a grinding aid containing waste liquid generated by caprolactam rearrangement reaction, which comprises the waste liquid generated by the caprolactam rearrangement reaction, modified sepiolite and a modified grinding aid; adding sepiolite powder into hydrochloric acid, stirring for 1-2h at 50-60 ℃, adding microcrystalline cellulose and ferric chloride, carrying out hydrothermal reaction for 10-18h at 180-200 ℃, filtering, washing for 2-4 times with deionized water, drying to constant weight at 100-110 ℃, and crushing to obtain the modified sepiolite. The invention has the advantages of easily obtained raw materials, low price, greatly reduced product cost, obvious grinding aiding effect, capability of reducing the distribution of cement particles and improving the strength of cement, simple and easy preparation method, mild reaction conditions, capability of storing the product for a long time, low requirement on reaction equipment and suitability for industrial production.
Description
Technical Field
The invention relates to the technical field of cement grinding aids, in particular to a grinding aid containing waste liquid generated by caprolactam rearrangement reaction and application thereof.
Background
In the cement production process, the power consumption for grinding is very high, and data shows that the utilization rate of energy in the cement grinding stage is extremely low, energy loss of 95-99 percent exists, and a method for thoroughly solving the problem does not exist at home and abroad, so that the application of the grinding aid becomes one of the main means for improving the grinding efficiency, improving the cement performance, saving energy, reducing consumption and reducing cost in the current cement industrial production.
The cement grinding aid is a chemical additive for improving the grinding effect and performance of cement, can be adsorbed on the surface of cement particles, plays a role in physical and chemical actions, can improve the machine-hour output of the cement under the condition of keeping the fineness of the ground cement and the power of a grinding machine unchanged, or can increase the specific surface area of the cement and improve the particle size grading of the ground cement under the condition of keeping the output of the cement and the power of the grinding machine unchanged, thereby improving the quality indexes of the cement such as strength and the like. In addition, the method can also obviously reduce energy consumption, improve the fluidity of the industrial waste residue, improve the utilization rate of the industrial waste residue and reduce environmental pollution, and has greater economic and social benefits and good development prospect.
At present, the main components of the grinding aid applied commercially are amine organic matters, polyalcohol organic matters and inorganic salts, the grinding aid compounded by a plurality of small molecular substances has a plurality of defects in use, the grinding aid capacity has an upper limit, the particle distribution range of a cement product is wide, the product is coarse, the cement strength is reduced, and even the cement strength grade is influenced.
At present, because caprolactam production technology is longer, production workshop sections are more, and the accessory substance is also more, and single technique is difficult to realize degrading all organic matters in the waste water, domestic current caprolactam waste water treatment generally adopts the method of multiple technical combination to handle, and not only the process is complicated, and the processing energy consumption is high, how to use the waste liquid that caprolactam rearrangement reaction produced for grinding aid to reduce cement particle distribution, improve cement intensity, become the technical problem that awaits solution at present.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a grinding aid containing waste liquid generated by caprolactam rearrangement reaction.
The grinding aid containing waste liquid generated by caprolactam rearrangement comprises waste liquid generated by caprolactam rearrangement, modified sepiolite and a modified grinding aid; wherein the weight ratio of waste liquid generated by caprolactam rearrangement reaction, modified sepiolite and modified grinding aid is 100: 10-20: 1-5;
adding sepiolite powder into hydrochloric acid, stirring for 1-2h at 50-60 ℃, adding microcrystalline cellulose and ferric chloride, carrying out hydrothermal reaction for 10-18h at 180-200 ℃, filtering, washing for 2-4 times with deionized water, drying to constant weight at 100-110 ℃, and crushing to obtain modified sepiolite;
in the modified grinding aid, 2-6 parts of hyperbranched polyethyleneimine, 4-10 parts of triethanolamine oleate soap, 1-5 parts of ethylene glycol, 1-5 parts of sodium lignosulfonate and 1-5 parts of glycerol are uniformly mixed according to parts by weight to obtain the modified grinding aid.
Preferably, the concentration of hydrochloric acid is 0.8 to 1.5 mol/L.
Preferably, the weight ratio of the sepiolite powder to the hydrochloric acid to the microcrystalline cellulose to the ferric chloride is 10-20: 100-200: 5-15: 2-6.
Preferably, the sepiolite powder has a bulk density of from 0.185 to 0.194g/cm3The viscosity is 900-1150 MPa.s.
Preferably, the microcrystalline cellulose has an ultimate degree of polymerization of 150-300.
Preferably, in the modified grinding aid, the weight ratio of the hyperbranched polyethyleneimine to the triethanolamine oleic soap to the glycol to the sodium lignosulfonate to the glycerol is 3-5: 5-8: 2-4: 2-4: 2-4.
The preparation method of the grinding aid containing the waste liquid generated by the caprolactam rearrangement reaction, which is provided by the invention, is characterized in that the modified sepiolite, the modified grinding aid and the waste liquid generated by the caprolactam rearrangement reaction are uniformly mixed to obtain the grinding aid containing the waste liquid generated by the caprolactam rearrangement reaction.
The invention also provides application of the grinding aid containing the waste liquid generated by the rearrangement reaction of caprolactam in cement.
The technical effects of the invention are as follows:
in the modified sepiolite, after the sepiolite powder is treated by hydrochloric acid, microcrystalline cellulose and ferric chloride are added for hydrothermal reaction, so that the adsorption effect of the sepiolite can be effectively improved, the obtained modified sepiolite has excellent performance, and the inventor finds that the sepiolite powder can be synergistically acted with waste liquid generated by rearrangement reaction of a modified grinding aid and caprolactam, so that the grinding aid effect can be improved, the distribution of cement particles can be effectively reduced, the cement slurry is stirred and coagulated and hardened more compactly, the sepiolite powder has certain adsorption capacity and can be firmly adsorbed on the surface of cement clinker, the materials can not be bonded with each other, the sepiolite powder can quickly permeate into cracks of the particles, the grinding efficiency is further improved, and in addition, the modified grinding aid contains a large amount of hyperbranched structures, so that the separation of the cement powder particles in superfine grinding can be effectively inhibited, avoids the phenomena of ball sticking, wall hanging and electrostatic adsorption, improves the grinding capacity of the grinding machine, increases the specific surface area of fine powder, and has the functions of quick setting and high hydration speed.
The grinding aid disclosed by the invention has the advantages of easily available raw materials, low price, capability of greatly reducing the product cost, remarkable grinding aid effect, capability of reducing the distribution of cement particles and improving the cement strength, simple and feasible preparation method, mild reaction conditions, capability of storing the product for a long time, low requirement on reaction equipment and suitability for industrial production.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A grinding aid containing waste liquid generated by caprolactam rearrangement reaction comprises waste liquid generated by caprolactam rearrangement reaction, modified sepiolite and a modified grinding aid; wherein the weight ratio of waste liquid generated by caprolactam rearrangement reaction, modified sepiolite and modified grinding aid is 100: 10: 1;
adding 10kg of sepiolite powder into 100kg of hydrochloric acid with the concentration of 0.8mol/L, stirring for 1h at the temperature of 50 ℃, adding 5kg of microcrystalline cellulose and 2kg of ferric chloride, carrying out hydrothermal reaction for 10h at the temperature of 180 ℃, filtering, washing for 2 times by using deionized water, drying to constant weight at the temperature of 100 ℃, and crushing to obtain the modified sepiolite;
in the modified grinding aid, 2kg of hyperbranched polyethyleneimine, 4kg of triethanolamine oleate soap, 1kg of ethylene glycol, 1kg of sodium lignosulfonate and 1kg of glycerol are uniformly mixed to obtain the modified grinding aid;
and uniformly mixing the modified sepiolite, the modified grinding aid and the waste liquid generated by the caprolactam rearrangement reaction to obtain the grinding aid containing the waste liquid generated by the caprolactam rearrangement reaction.
Example 2
A grinding aid containing waste liquid generated by caprolactam rearrangement reaction comprises waste liquid generated by caprolactam rearrangement reaction, modified sepiolite and a modified grinding aid; wherein the weight ratio of waste liquid generated by caprolactam rearrangement reaction, modified sepiolite and modified grinding aid is 100: 20: 5;
adding 20kg of sepiolite powder into 200kg of hydrochloric acid with the concentration of 1.5mol/L, stirring for 2h at the temperature of 60 ℃, adding 15kg of microcrystalline cellulose and 6kg of ferric chloride, carrying out hydrothermal reaction for 18h at the temperature of 200 ℃, filtering, washing for 4 times by using deionized water, drying to constant weight at the temperature of 110 ℃, and crushing to obtain the modified sepiolite;
in the modified grinding aid, 6kg of hyperbranched polyethyleneimine, 10kg of triethanolamine oleate soap, 5kg of ethylene glycol, 5kg of sodium lignosulfonate and 5kg of glycerol are uniformly mixed to obtain the modified grinding aid;
and uniformly mixing the modified sepiolite, the modified grinding aid and the waste liquid generated by the caprolactam rearrangement reaction to obtain the grinding aid containing the waste liquid generated by the caprolactam rearrangement reaction.
Example 3
A grinding aid containing waste liquid generated by caprolactam rearrangement reaction comprises waste liquid generated by caprolactam rearrangement reaction, modified sepiolite and a modified grinding aid; wherein the weight ratio of waste liquid generated by caprolactam rearrangement reaction, modified sepiolite and modified grinding aid is 100: 11: 2;
adding 12kg of sepiolite powder into 120kg of hydrochloric acid with the concentration of 1mol/L, stirring for 1.2h at the temperature of 54 ℃, adding 6kg of microcrystalline cellulose and 3kg of ferric chloride, carrying out hydrothermal reaction for 12h at the temperature of 185 ℃, filtering, washing for 3 times by using deionized water, drying to constant weight at the temperature of 102 ℃, and crushing to obtain the modified sepiolite;
in the modified grinding aid, 3kg of hyperbranched polyethyleneimine, 5kg of triethanolamine oleate soap, 2kg of ethylene glycol, 2kg of sodium lignosulfonate and 2kg of glycerol are uniformly mixed to obtain the modified grinding aid;
and uniformly mixing the modified sepiolite, the modified grinding aid and the waste liquid generated by the caprolactam rearrangement reaction to obtain the grinding aid containing the waste liquid generated by the caprolactam rearrangement reaction.
Example 4
A grinding aid containing waste liquid generated by caprolactam rearrangement reaction comprises waste liquid generated by caprolactam rearrangement reaction, modified sepiolite and a modified grinding aid; wherein the weight ratio of waste liquid generated by caprolactam rearrangement reaction, modified sepiolite and modified grinding aid is 100: 15: 3;
adding 15kg of sepiolite powder into 150kg of hydrochloric acid with the concentration of 1mol/L, stirring for 1.5h at the temperature of 55 ℃, adding 12kg of microcrystalline cellulose and 3kg of ferric chloride, carrying out hydrothermal reaction for 15h at the temperature of 190 ℃, filtering, washing for 3 times by using deionized water, drying to constant weight at the temperature of 105 ℃, and crushing to obtain the modified sepiolite;
in the modified grinding aid, 4kg of hyperbranched polyethyleneimine, 6kg of triethanolamine oleate soap, 2kg of ethylene glycol, 3kg of sodium lignosulfonate and 3kg of glycerol are uniformly mixed to obtain the modified grinding aid;
and uniformly mixing the modified sepiolite, the modified grinding aid and the waste liquid generated by the caprolactam rearrangement reaction to obtain the grinding aid containing the waste liquid generated by the caprolactam rearrangement reaction.
Example 5
A grinding aid containing waste liquid generated by caprolactam rearrangement reaction comprises waste liquid generated by caprolactam rearrangement reaction, modified sepiolite and a modified grinding aid; wherein the weight ratio of waste liquid generated by caprolactam rearrangement reaction, modified sepiolite and modified grinding aid is 100: 18: 4;
adding 18kg of sepiolite powder into 192kg of hydrochloric acid with the concentration of 1.3mol/L, stirring for 1.8h at the temperature of 58 ℃, adding 12kg of microcrystalline cellulose and 4kg of ferric chloride, carrying out hydrothermal reaction for 17h at the temperature of 193 ℃, filtering, washing for 3 times by deionized water, drying to constant weight at the temperature of 108 ℃, and crushing to obtain the modified sepiolite;
in the modified grinding aid, 5kg of hyperbranched polyethyleneimine, 8kg of triethanolamine oleate soap, 3kg of ethylene glycol, 4kg of sodium lignosulfonate and 4kg of glycerol are uniformly mixed to obtain the modified grinding aid;
and uniformly mixing the modified sepiolite, the modified grinding aid and the waste liquid generated by the caprolactam rearrangement reaction to obtain the grinding aid containing the waste liquid generated by the caprolactam rearrangement reaction.
Comparative example 1
A grinding aid containing waste liquid generated by caprolactam rearrangement reaction comprises the waste liquid generated by the caprolactam rearrangement reaction and a modified grinding aid; wherein the weight ratio of waste liquid generated by caprolactam rearrangement reaction to the modified grinding aid is 100: 4;
in the modified grinding aid, 5kg of hyperbranched polyethyleneimine, 8kg of triethanolamine oleate soap, 3kg of ethylene glycol, 4kg of sodium lignosulfonate and 4kg of glycerol are uniformly mixed to obtain the modified grinding aid;
and uniformly mixing the modified grinding aid and the waste liquid generated by the caprolactam rearrangement reaction to obtain the grinding aid containing the waste liquid generated by the caprolactam rearrangement reaction.
Comparative example 2
A grinding aid containing waste liquid generated by caprolactam rearrangement reaction comprises waste liquid generated by caprolactam rearrangement reaction and modified sepiolite; wherein the weight ratio of waste liquid generated by caprolactam rearrangement reaction, modified sepiolite and modified grinding aid is 100: 18;
adding 18kg of sepiolite powder into 192kg of hydrochloric acid with the concentration of 1.3mol/L, stirring for 1.8h at the temperature of 58 ℃, adding 12kg of microcrystalline cellulose and 4kg of ferric chloride, carrying out hydrothermal reaction for 17h at the temperature of 193 ℃, filtering, washing for 3 times by deionized water, drying to constant weight at the temperature of 108 ℃, and crushing to obtain the modified sepiolite;
and uniformly mixing the modified sepiolite and the waste liquid generated by the rearrangement reaction of caprolactam to obtain the grinding aid containing the waste liquid generated by the rearrangement reaction of caprolactam.
The grinding aids of example 5, comparative example 1 and comparative example 2 were tested, and the test results are shown below:
test items | Example 5 | Example 4 | Example 3 |
Stability of | Qualified | Qualified | Qualified |
Specific surface area m2/kg | 368 | 393 | 405 |
Fineness% | 3.8 | 3.7 | 3.9 |
Standard consistency% | 120.5 | 119.4 | 118.2 |
The grinding aids of example 5, comparative example 1 and comparative example 2 are applied to cement clinker, the addition amount is 0.6 wt%, the mechanical properties of the cement are detected, and the detection results are as follows:
test items | Example 5 | Example 4 | Example 3 |
3d flexural strength MPa | 35 | 29 | 27 |
7d flexural strength MPa | 49 | 43 | 46 |
28d flexural strength MPa | 60 | 56 | 55 |
3d compressive strength MPa | 5.9 | 5.7 | 5.6 |
7d compressive strength MPa | 8.5 | 8.4 | 8.2 |
28d compressive strength MPa | 9.8 | 9.5 | 9.7 |
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. A grinding aid containing waste liquid generated by caprolactam rearrangement reaction is characterized by comprising the waste liquid generated by the caprolactam rearrangement reaction, modified sepiolite and a modified grinding aid; wherein the weight ratio of waste liquid generated by caprolactam rearrangement reaction, modified sepiolite and modified grinding aid is 100: 10-20: 1-5;
adding sepiolite powder into hydrochloric acid, stirring for 1-2h at 50-60 ℃, adding microcrystalline cellulose and ferric chloride, carrying out hydrothermal reaction for 10-18h at 180-200 ℃, filtering, washing for 2-4 times with deionized water, drying to constant weight at 100-110 ℃, and crushing to obtain modified sepiolite;
in the modified grinding aid, 2-6 parts of hyperbranched polyethyleneimine, 4-10 parts of triethanolamine oleate soap, 1-5 parts of ethylene glycol, 1-5 parts of sodium lignosulfonate and 1-5 parts of glycerol are uniformly mixed according to parts by weight to obtain the modified grinding aid.
2. The grinding aid containing waste liquid generated by caprolactam rearrangement reaction according to claim 1, wherein the concentration of hydrochloric acid is 0.8-1.5 mol/L.
3. The grinding aid containing waste liquid generated by caprolactam rearrangement reaction according to claim 1, wherein the weight ratio of sepiolite powder, hydrochloric acid, microcrystalline cellulose and ferric chloride is 10-20: 100-200: 5-15: 2-6.
4. The grinding aid containing waste liquid generated by caprolactam rearrangement reaction according to claim 1, wherein the sepiolite powder has a bulk density of 0.185 to 0.194g/cm3The viscosity is 900-1150 MPa.s.
5. The grinding aid containing waste liquid generated by caprolactam rearrangement reaction of claim 1, wherein the limiting degree of polymerization of the microcrystalline cellulose is 150-300.
6. The grinding aid containing waste liquid generated by caprolactam rearrangement reaction according to claim 1, wherein in the modified grinding aid, the weight ratio of the hyperbranched polyethyleneimine, the triethanolamine oleate soap, the glycol, the sodium lignin sulfonate and the glycerol is 3-5: 5-8: 2-4: 2-4: 2-4.
7. A preparation method of a grinding aid containing waste liquid generated by caprolactam rearrangement reaction according to any one of claims 1 to 6, characterized in that the modified sepiolite, the modified grinding aid and the waste liquid generated by the caprolactam rearrangement reaction are uniformly mixed to obtain the grinding aid containing the waste liquid generated by the caprolactam rearrangement reaction.
8. Use of a grinding aid comprising a waste stream from a caprolactam rearrangement reaction according to any one of claims 1 to 6 in cement.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113698126A (en) * | 2021-10-13 | 2021-11-26 | 广州基业长青新材料有限公司 | Efficient cement grinding aid and preparation method and application thereof |
CN115041253A (en) * | 2022-06-01 | 2022-09-13 | 成都进达科技有限公司 | Raw material coal-saving auxiliary agent for cement clinker firing process and preparation method thereof |
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2021
- 2021-03-02 CN CN202110230119.8A patent/CN112919845A/en not_active Withdrawn
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113698126A (en) * | 2021-10-13 | 2021-11-26 | 广州基业长青新材料有限公司 | Efficient cement grinding aid and preparation method and application thereof |
CN115041253A (en) * | 2022-06-01 | 2022-09-13 | 成都进达科技有限公司 | Raw material coal-saving auxiliary agent for cement clinker firing process and preparation method thereof |
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