Preparation method of cement grinding aid

文档序号:823635 发布日期:2021-03-30 浏览:30次 中文

阅读说明:本技术 一种水泥助磨剂的制备方法 (Preparation method of cement grinding aid ) 是由 王彦明 于 2020-12-31 设计创作,主要内容包括:本发明涉及水泥助磨技术领域,尤其涉及一种水泥助磨剂的制备方法,解决了现有技术中水泥助磨剂的产品性能波动大,其能提高粉磨的效率一般,影响了其助磨增强性能的发挥的缺点,包括以下成分:烟秆黑液、磺化剂、废糖蜜、三乙醇胺、黄酮、木质素磺酸钠、增稠剂、柠檬苦素、硫酸钠溶液、水。本发明通过烟秆黑液为部分原料,对其处理后进行再利用组成水泥助磨剂,降低成本,且通过分级处理得到各部分的溶液,并对其分别进行不同温度、不同步骤的处理,最终得到溶液B及溶液D,再将二者在边加入边搅拌的条件下进行混匀处理,最终通过加入增稠剂来提高水泥助磨剂的粘稠性,得到质量较佳的水泥助磨剂。(The invention relates to the technical field of cement grinding aid, in particular to a preparation method of a cement grinding aid, which solves the defects that the product performance of the cement grinding aid in the prior art is large in fluctuation, the grinding efficiency can be improved generally, and the performance of the grinding-aid enhancing performance is influenced, and comprises the following components: the tobacco stem black liquor, a sulfonating agent, waste molasses, triethanolamine, flavone, sodium lignosulfonate, a thickening agent, limonin, a sodium sulfate solution and water. According to the invention, the tobacco stem black liquor is used as a part of raw materials, the treated tobacco stem black liquor is recycled to form the cement grinding aid, the cost is reduced, the solutions of each part are obtained through grading treatment, the solutions are respectively treated at different temperatures and in different steps to finally obtain the solution B and the solution D, the solution B and the solution D are uniformly mixed under the condition of adding and stirring, and finally the thickening agent is added to improve the viscosity of the cement grinding aid, so that the cement grinding aid with better quality is obtained.)

1. The cement grinding aid is characterized by comprising the following components in parts by weight: 100-200 parts of tobacco stem black liquor, 10-20 parts of sulfonating agent, 90-120 parts of waste molasses, 80-100 parts of triethanolamine, 40-80 parts of flavone, 60-100 parts of sodium lignosulfonate, 30-50 parts of thickening agent, 30-70 parts of limonin, 40-80 parts of sodium sulfate solution and 120-200 parts of water.

2. The cement grinding aid as claimed in claim 1, which is characterized by comprising the following components in parts by weight: 150 parts of black tobacco stem liquor, 12 parts of sulfonating agent, 110 parts of waste molasses, 90 parts of triethanolamine, 60 parts of flavone, 80 parts of sodium lignosulfonate, 40 parts of thickening agent, 50 parts of limonin, 60 parts of sodium sulfate solution and 140 parts of water.

3. The cement grinding aid as claimed in claim 1 or 2, wherein the thickener is one or more of hydroxypropyl methylcellulose and hydroxyethyl cellulose.

4. A cement grinding aid as claimed in claim 1 or 2 wherein said sulfonating agent is one or more of ammonium bisulfite, sulfuric acid, sodium sulfite.

5. A method for preparing a cement grinding aid according to any one of claims 1 to 4, characterized by comprising the following steps:

s1: taking the tobacco stem black liquor, and adjusting the pH value of the tobacco stem black liquor to 9-10 by using a sodium hydroxide or hydrochloric acid solution for later use;

s2: adding the sulfonating agent into the treatment solution of S1, continuously reacting at 60-80 ℃ for 150-240 min, then carrying out spray drying to obtain tobacco stem black liquor powder, and standing for later use;

s3: adding half of the water into a mixing kettle, then adding the waste molasses and the triethanolamine according to a proportion, and continuously stirring until the mixture is uniform to obtain a solution A;

s4: adjusting the temperature of the mixing kettle to 35-40 ℃, adding the tobacco stem black liquor powder in the S2 into the mixing kettle, continuously stirring for 10-20 min, heating to 50-60 ℃, adding flavone, and continuously stirring for 20-30 min to obtain a solution B;

s5: adding sodium lignosulfonate and sodium sulfate solution into the other half of the water in a reaction kettle, sealing the reaction kettle, carrying out condensation reaction for 4-8 hours, and cooling to room temperature to obtain solution C;

s6: adjusting the temperature of the reaction kettle to 40-45 ℃, then adding limonin into the solution C, and continuously stirring for 15-20 min until the solution C is uniform, so as to obtain a solution D;

s7: adding the solution D into the solution B, stirring while adding, and keeping the temperature at 45-50 ℃ until the solution is uniform to obtain a solution E;

s8: and adding a thickening agent into the solution E, keeping the temperature at 30-40 ℃, and stirring for 15-20 min until the solution is uniform to obtain the finished cement grinding aid.

6. The method for preparing the cement grinding aid according to claim 5, wherein in S2, the temperature of an atomizer of a spray drying device is 160-300 ℃, and the temperature of a spray outlet is 75-90 ℃.

7. The method for preparing the cement grinding aid according to claim 5, wherein in S4, the temperature of a mixing kettle is adjusted to 37 ℃, then the tobacco stalk black liquor powder in S2 is added into the mixing kettle, the stirring is continued for 15min, then the temperature is increased to 55 ℃, the flavone is added, and the stirring is continued for 25min, so that a solution B is obtained.

8. The preparation method of the cement grinding aid as claimed in claim 5, wherein in S5, the condensation reaction temperature is 90-110 ℃, and the pressure is controlled at 1.0-2.0 MPa.

9. A use method of the cement grinding aid according to any one of claims 1 to 4, characterized in that the cement grinding aid is directly used in the cement grinding process according to 0.03 to 0.05 percent of the total mass of the cement.

Technical Field

The invention relates to the technical field of cement grinding aid, in particular to a preparation method of a cement grinding aid.

Background

Cement is the most commonly used building material and is widely applied to civil construction, hydraulic power, national defense and other projects, a mill is needed to grind the cement into powder in the processing process, and a cement grinding aid is added in the process to improve the early strength and the later strength of the cement.

The cement grinding aid is a chemical additive for improving the grinding effect and performance of cement, can obviously improve the machine-hour output of cement and the strength of cement at each age, and improves the fluidity of the cement. However, the performance of the existing cement grinding aid has large fluctuation, the grinding efficiency can be improved, and the performance of the grinding-aid reinforcing performance is influenced.

Therefore, we propose a method for preparing a cement grinding aid to solve the above problems.

Disclosure of Invention

The invention aims to solve the defects in the prior art and provides a preparation method of a cement grinding aid.

In order to achieve the purpose, the invention adopts the following technical scheme:

the invention provides a cement grinding aid which comprises the following components in parts by weight: 100-200 parts of tobacco stem black liquor, 10-20 parts of sulfonating agent, 90-120 parts of waste molasses, 80-100 parts of triethanolamine, 40-80 parts of flavone, 60-100 parts of sodium lignosulfonate, 30-50 parts of thickening agent, 30-70 parts of limonin, 40-80 parts of sodium sulfate solution and 120-200 parts of water.

Preferably, the cement grinding aid comprises the following components in parts by weight: 150 parts of black tobacco stem liquor, 12 parts of sulfonating agent, 110 parts of waste molasses, 90 parts of triethanolamine, 60 parts of flavone, 80 parts of sodium lignosulfonate, 40 parts of thickening agent, 50 parts of limonin, 60 parts of sodium sulfate solution and 140 parts of water.

Preferably, the thickener is one or more of hydroxypropyl methylcellulose and hydroxyethyl cellulose.

Preferably, the sulfonating agent is one or more of ammonium bisulfite, sulfuric acid and sodium sulfite.

Preferably, the preparation method of the cement grinding aid comprises the following steps:

s1: taking the tobacco stem black liquor, and adjusting the pH value of the tobacco stem black liquor to 9-10 by using a sodium hydroxide or hydrochloric acid solution for later use;

s2: adding the sulfonating agent into the treatment solution of S1, continuously reacting at 60-80 ℃ for 150-240 min, then carrying out spray drying to obtain tobacco stem black liquor powder, and standing for later use;

s3: adding half of the water into a mixing kettle, then adding the waste molasses and the triethanolamine according to a proportion, and continuously stirring until the mixture is uniform to obtain a solution A;

s4: adjusting the temperature of the mixing kettle to 35-40 ℃, adding the tobacco stem black liquor powder in the S2 into the mixing kettle, continuously stirring for 10-20 min, heating to 50-60 ℃, adding flavone, and continuously stirring for 20-30 min to obtain a solution B;

s5: adding the sodium lignosulfonate sodium sulfate solution into the other half of the water in a reaction kettle, sealing the reaction kettle, carrying out condensation reaction for 4-8 hours, and cooling to room temperature to obtain a solution C;

s6: adjusting the temperature of the reaction kettle to 40-45 ℃, then adding limonin into the solution C, and continuously stirring for 15-20 min until the solution C is uniform, so as to obtain a solution D;

s7: adding the solution D into the solution B, stirring while adding, and keeping the temperature at 45-50 ℃ until the solution is uniform to obtain a solution E;

s8: and adding a thickening agent into the solution E, keeping the temperature at 30-40 ℃, and stirring for 15-20 min until the solution is uniform to obtain the finished cement grinding aid.

Preferably, in S2, the temperature of an atomizer of the spray drying equipment is 160-300 ℃, and the temperature of a spray outlet is 75-90 ℃.

Preferably, in the step S4, the temperature of the mixing kettle is adjusted to 37 ℃, then the tobacco stem black liquor powder in the step S2 is added into the mixing kettle, continuously stirred for 15min, then heated to 55 ℃, added with flavone, and continuously stirred for 25min, so as to obtain a solution B.

Preferably, in the S5, the condensation reaction temperature is 90-110 ℃, and the pressure is controlled to be 1.0-2.0 MPa.

Preferably, the application method of the cement grinding aid is characterized in that the cement grinding aid is directly used in the cement grinding process according to 0.03-0.05 percent of the total mass of cement.

Compared with the prior art, the invention has the beneficial effects that:

1. according to the invention, the tobacco stem black liquor is used as a part of raw materials, the processed tobacco stem black liquor is recycled to form the cement grinding aid, and in the process of uniformly mixing the waste molasses, the triethanolamine and the tobacco stem black liquor, the flavone is added for pretreatment to obtain the processing liquor, so that the mutual attraction of uniformly mixed substances is increased, the subsequent uniform mixing effect is promoted, the obtained cement grinding aid has good quality, and the grinding efficiency and quality of a grinding machine can be effectively improved.

2. The invention integrates sodium lignosulfonate and sodium sulfate to prepare another mixed solution to obtain a solution C, the solution C is prepared by grading and dividing the temperature, the mixing efficiency of all the substances is high, the limonin is added at the regulated temperature, and the finally obtained cement grinding aid can greatly improve the compression resistance of the finished concrete in the application process.

3. According to the invention, the solutions of each part are obtained through grading treatment, the solutions are respectively treated at different temperatures and in different steps to finally obtain the solution B and the solution D, the solution B and the solution D are uniformly mixed under the condition of adding and stirring, and finally the thickening agent is added to improve the viscosity of the cement grinding aid to obtain the cement grinding aid with better quality.

Detailed Description

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control. When "mass, concentration, temperature, time, or other value or parameter is expressed as a range, preferred range, or as a range defined by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, a range of 1 to 50 should be understood to include any number, combination of numbers, or subrange selected from 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, or 50, and all fractional values between the above integers, e.g., 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, and 1.9. With respect to sub-ranges, specifically consider "nested sub-ranges" that extend from any endpoint within the range. For example, nested sub-ranges of exemplary ranges 1-50 may include 1-10, 1-20, 1-30, and 1-40 in one direction, or 50-40, 50-30, 50-20, and 50-10 in another direction. "

The present invention is further illustrated below with reference to specific examples in which various processes and methods not described in detail are conventional methods well known in the art. Materials, reagents, devices, instruments, apparatuses and the like used in the following examples are commercially available unless otherwise specified.

Example one

The invention provides a cement grinding aid which comprises the following components in parts by weight: 100 parts of black tobacco stem liquor, 10 parts of sulfonating agent, 90 parts of waste molasses, 80 parts of triethanolamine, 40 parts of flavone, 60 parts of sodium lignosulfonate, 30 parts of thickening agent, 30 parts of limonin, 40 parts of sodium sulfate solution and 120 parts of water.

Wherein, the thickening agent is one or more of hydroxypropyl methylcellulose and hydroxyethyl cellulose, and the sulfonating agent is one or more of ammonium bisulfite, sulfuric acid and sodium sulfite.

In the embodiment, the preparation method of the cement grinding aid is also provided, and comprises the following steps:

s1: taking the tobacco stalk black liquor, and adjusting the pH value to 9 in the tobacco stalk black liquor by using a sodium hydroxide or hydrochloric acid solution for later use;

s2: adding the sulfonating agent into the treatment solution of S1, continuously reacting at 60 ℃ for 150min, then spray-drying at 160 ℃ of an atomizer of spray-drying equipment and 75 ℃ of a spray outlet to obtain tobacco stem black liquor powder, and standing for later use;

s3: adding half of the water into a mixing kettle, then adding the waste molasses and the triethanolamine according to a proportion, and continuously stirring until the mixture is uniform to obtain a solution A;

s4: adjusting the temperature of the mixing kettle to 35 ℃, adding the tobacco stem black liquor powder in the S2 into the mixing kettle, continuously stirring for 10min, then heating to 50 ℃, adding flavone, and continuously stirring for 20min to obtain a solution B;

s5: adding sodium lignosulfonate and sodium sulfate solution into the other half of the water in a reaction kettle, sealing the reaction kettle, carrying out condensation reaction at 90 ℃, controlling the pressure at 1.0MPa for 4 hours, and cooling to room temperature to obtain solution C;

s6: adjusting the temperature of the reaction kettle to 40 ℃, adding limonin into the solution C, and continuously stirring for 15min until the solution C is uniform, so as to obtain a solution D;

s7: adding the solution D into the solution B, stirring while adding, and keeping the temperature at 45 ℃ until the solution is uniform to obtain a solution E;

s8: and adding a thickening agent into the solution E, keeping the temperature at 30 ℃, and stirring for 15min until the solution is uniform to obtain the finished cement grinding aid.

Specifically, the method also comprises a using method of the cement grinding aid, wherein the cement grinding aid is directly used in the cement grinding process according to 0.03-0.05 percent of the total mass of the cement.

Example two

The invention provides a cement grinding aid which comprises the following components in parts by weight: 120 parts of tobacco stem black liquor, 14 parts of sulfonating agent, 100 parts of waste molasses, 85 parts of triethanolamine, 50 parts of flavone, 70 parts of sodium lignosulfonate, 35 parts of thickening agent, 40 parts of limonin, 50 parts of sodium sulfate solution and 140 parts of water.

Wherein, the thickening agent is one or more of hydroxypropyl methylcellulose and hydroxyethyl cellulose, and the sulfonating agent is one or more of ammonium bisulfite, sulfuric acid and sodium sulfite.

In the embodiment, the preparation method of the cement grinding aid is also provided, and comprises the following steps:

s1: taking the tobacco stalk black liquor, and adjusting the pH value to 9 in the tobacco stalk black liquor by using a sodium hydroxide or hydrochloric acid solution for later use;

s2: adding the sulfonating agent into the treatment solution of S1, continuously reacting at 65 ℃ for 170min, then spray-drying, wherein the temperature of an atomizer of spray-drying equipment is 180 ℃, and the temperature of a spray outlet is 80 ℃ to obtain tobacco stem black liquor powder, and standing for later use;

s3: adding half of the water into a mixing kettle, then adding the waste molasses and the triethanolamine according to a proportion, and continuously stirring until the mixture is uniform to obtain a solution A;

s4: adjusting the temperature of the mixing kettle to 37 ℃, adding the tobacco stem black liquor powder in the S2 into the mixing kettle, continuously stirring for 14min, heating to 54 ℃, adding flavone, and continuously stirring for 24min to obtain a solution B;

s5: adding sodium lignosulfonate and sodium sulfate solution into the other half of the water in a reaction kettle, sealing the reaction kettle, carrying out condensation reaction at the temperature of 95 ℃, controlling the pressure to be 1.5MPa for 5 hours, and cooling to room temperature to obtain solution C;

s6: adjusting the temperature of the reaction kettle to 42 ℃, adding limonin into the solution C, and continuously stirring for 17min until the solution C is uniform, so as to obtain a solution D;

s7: adding the solution D into the solution B, stirring while adding, and keeping the temperature at 47 ℃ until the solution is uniform to obtain a solution E;

s8: and adding a thickening agent into the solution E, keeping the temperature at 35 ℃, and stirring for 17min until the solution is uniform to obtain the finished cement grinding aid.

Specifically, the method also comprises a using method of the cement grinding aid, wherein the cement grinding aid is directly used in the cement grinding process according to 0.03-0.05 percent of the total mass of the cement.

EXAMPLE III

The invention provides a cement grinding aid which comprises the following components in parts by weight: 180 parts of black tobacco stem liquor, 18 parts of sulfonating agent, 110 parts of waste molasses, 95 parts of triethanolamine, 70 parts of flavone, 90 parts of sodium lignosulfonate, 45 parts of thickening agent, 60 parts of limonin, 70 parts of sodium sulfate solution and 180 parts of water.

Wherein, the thickening agent is one or more of hydroxypropyl methylcellulose and hydroxyethyl cellulose, and the sulfonating agent is one or more of ammonium bisulfite, sulfuric acid and sodium sulfite.

In the embodiment, the preparation method of the cement grinding aid is also provided, and comprises the following steps:

s1: taking the tobacco stalk black liquor, and adjusting the pH value of the tobacco stalk black liquor to 10 by using a sodium hydroxide or hydrochloric acid solution for later use;

s2: adding the sulfonating agent into the treatment solution of S1, continuously reacting at 75 ℃ for 220min, then spray-drying, wherein the temperature of an atomizer of spray-drying equipment is 250 ℃, and the temperature of a spray outlet is 85 ℃ to obtain tobacco stem black liquor powder, and standing for later use;

s3: adding half of the water into a mixing kettle, then adding the waste molasses and the triethanolamine according to a proportion, and continuously stirring until the mixture is uniform to obtain a solution A;

s4: adjusting the temperature of the mixing kettle to 39 ℃, adding the tobacco stem black liquor powder in the S2 into the mixing kettle, continuously stirring for 18min, then heating to 58 ℃, adding flavone, and continuously stirring for 28min to obtain a solution B;

s5: adding sodium lignosulfonate and sodium sulfate solution into the other half of the water in a reaction kettle, sealing the reaction kettle, carrying out condensation reaction at 105 ℃, controlling the pressure at 2.0MPa for 7 hours, and cooling to room temperature to obtain solution C;

s6: adjusting the temperature of the reaction kettle to 45 ℃, adding limonin into the solution C, and continuously stirring for 18min until the solution C is uniform, so as to obtain a solution D;

s7: adding the solution D into the solution B, stirring while adding, and keeping the temperature at 48 ℃ until the solution is uniform to obtain a solution E;

s8: and adding a thickening agent into the solution E, keeping the temperature at 38 ℃, and stirring for 18min until the solution is uniform to obtain the finished cement grinding aid.

Specifically, the method also comprises a using method of the cement grinding aid, wherein the cement grinding aid is directly used in the cement grinding process according to 0.03-0.05 percent of the total mass of the cement.

Example four

The invention provides a cement grinding aid which comprises the following components in parts by weight: 200 parts of black tobacco stem liquor, 20 parts of sulfonating agent, 120 parts of waste molasses, 100 parts of triethanolamine, 80 parts of flavone, 100 parts of sodium lignosulfonate, 50 parts of thickening agent, 70 parts of limonin, 80 parts of sodium sulfate solution and 200 parts of water.

Wherein, the thickening agent is one or more of hydroxypropyl methylcellulose and hydroxyethyl cellulose, and the sulfonating agent is one or more of ammonium bisulfite, sulfuric acid and sodium sulfite.

In the embodiment, the preparation method of the cement grinding aid is also provided, and comprises the following steps:

s1: taking the tobacco stalk black liquor, and adjusting the pH value of the tobacco stalk black liquor to 10 by using a sodium hydroxide or hydrochloric acid solution for later use;

s2: adding the sulfonating agent into the treatment solution of S1, carrying out continuous reaction at 80 ℃, carrying out continuous reaction for 240min, then carrying out spray drying, wherein the temperature of an atomizer of the spray drying equipment is 300 ℃, and the temperature of a spray outlet is 90 ℃, so as to obtain tobacco stem black liquor powder, and placing for later use;

s3: adding half of the water into a mixing kettle, then adding the waste molasses and the triethanolamine according to a proportion, and continuously stirring until the mixture is uniform to obtain a solution A;

s4: adjusting the temperature of the mixing kettle to 40 ℃, adding the tobacco stem black liquor powder in the S2 into the mixing kettle, continuously stirring for 20min, then heating to 60 ℃, adding flavone, and continuously stirring for 30min to obtain a solution B;

s5: adding sodium lignosulfonate and sodium sulfate solution into the other half of the water in a reaction kettle, sealing the reaction kettle, carrying out condensation reaction at 110 ℃, controlling the pressure at 2.0MPa for 8 hours, and cooling to room temperature to obtain solution C;

s6: adjusting the temperature of the reaction kettle to 45 ℃, adding limonin into the solution C, and continuously stirring for 20min until the solution C is uniform, so as to obtain a solution D;

s7: adding the solution D into the solution B, stirring while adding, and keeping the temperature at 50 ℃ until the solution is uniform to obtain a solution E;

s8: and adding a thickening agent into the solution E, keeping the temperature at 40 ℃, and stirring for 20min until the solution is uniform to obtain the finished cement grinding aid.

Specifically, the method also comprises a using method of the cement grinding aid, wherein the cement grinding aid is directly used in the cement grinding process according to 0.03-0.05 percent of the total mass of the cement.

Comparative example 1

The cement grinding aid comprises the following components in parts by weight: 200 parts of tobacco stem black liquor, 20 parts of sulfonating agent, 120 parts of waste molasses, 100 parts of triethanolamine, 100 parts of sodium lignosulfonate, 50 parts of thickening agent, 70 parts of limonin, 80 parts of sodium sulfate solution and 200 parts of water.

Wherein, the thickening agent is one or more of hydroxypropyl methylcellulose and hydroxyethyl cellulose, and the sulfonating agent is one or more of ammonium bisulfite, sulfuric acid and sodium sulfite.

In the comparative example, a preparation method of the cement grinding aid is also provided, and the preparation method comprises the following steps:

s1: taking the tobacco stalk black liquor, and adjusting the pH value of the tobacco stalk black liquor to 10 by using a sodium hydroxide or hydrochloric acid solution for later use;

s2: adding the sulfonating agent into the treatment solution of S1, carrying out continuous reaction at 80 ℃, carrying out continuous reaction for 240min, then carrying out spray drying, wherein the temperature of an atomizer of the spray drying equipment is 300 ℃, and the temperature of a spray outlet is 90 ℃, so as to obtain tobacco stem black liquor powder, and placing for later use;

s3: adding half of the water into a mixing kettle, then adding the waste molasses and the triethanolamine according to a proportion, and continuously stirring until the mixture is uniform to obtain a solution A;

s4: adjusting the temperature of the mixing kettle to 40 ℃, adding the tobacco stem black liquor powder in the S2 into the mixing kettle, and continuously stirring for 20min to obtain a solution B;

s5: adding sodium lignosulfonate and sodium sulfate solution into the other half of the water in a reaction kettle, sealing the reaction kettle, carrying out condensation reaction at 110 ℃, controlling the pressure at 2.0MPa for 8 hours, and cooling to room temperature to obtain solution C;

s6: adjusting the temperature of the reaction kettle to 45 ℃, adding limonin into the solution C, and continuously stirring for 20min until the solution C is uniform, so as to obtain a solution D;

s7: adding the solution D into the solution B, stirring while adding, and keeping the temperature at 50 ℃ until the solution is uniform to obtain a solution E;

s8: and adding a thickening agent into the solution E, keeping the temperature at 40 ℃, and stirring for 20min until the solution is uniform to obtain the finished cement grinding aid.

Specifically, the method also comprises a using method of the cement grinding aid, wherein the cement grinding aid is directly used in the cement grinding process according to 0.03-0.05 percent of the total mass of the cement.

Comparative example No. two

The cement grinding aid comprises the following components in parts by weight: 200 parts of black tobacco stem liquor, 20 parts of sulfonating agent, 120 parts of waste molasses, 100 parts of triethanolamine, 80 parts of flavone, 100 parts of sodium lignosulfonate, 50 parts of thickening agent, 80 parts of sodium sulfate solution and 200 parts of water.

Wherein, the thickening agent is one or more of hydroxypropyl methylcellulose and hydroxyethyl cellulose, and the sulfonating agent is one or more of ammonium bisulfite, sulfuric acid and sodium sulfite.

In the comparative example, a preparation method of the cement grinding aid is also provided, and the preparation method comprises the following steps:

s1: taking the tobacco stalk black liquor, and adjusting the pH value of the tobacco stalk black liquor to 10 by using a sodium hydroxide or hydrochloric acid solution for later use;

s2: adding the sulfonating agent into the treatment solution of S1, carrying out continuous reaction at 80 ℃, carrying out continuous reaction for 240min, then carrying out spray drying, wherein the temperature of an atomizer of the spray drying equipment is 300 ℃, and the temperature of a spray outlet is 90 ℃, so as to obtain tobacco stem black liquor powder, and placing for later use;

s3: adding half of the water into a mixing kettle, then adding the waste molasses and the triethanolamine according to a proportion, and continuously stirring until the mixture is uniform to obtain a solution A;

s4: adjusting the temperature of the mixing kettle to 40 ℃, adding the tobacco stem black liquor powder in the S2 into the mixing kettle, continuously stirring for 20min, then heating to 60 ℃, adding flavone, and continuously stirring for 30min to obtain a solution B;

s5: adding sodium lignosulfonate and sodium sulfate solution into the other half of the water in a reaction kettle, sealing the reaction kettle, carrying out condensation reaction at 110 ℃, controlling the pressure at 2.0MPa for 8 hours, and cooling to room temperature to obtain solution C;

s6: adding the solution C into the solution B, stirring while adding, and keeping the temperature at 50 ℃ until the solution is uniform to obtain a solution E;

s7: and adding a thickening agent into the solution E, keeping the temperature at 40 ℃, and stirring for 20min until the solution is uniform to obtain the finished cement grinding aid.

Specifically, the method also comprises a using method of the cement grinding aid, wherein the cement grinding aid is directly used in the cement grinding process according to 0.03-0.05 percent of the total mass of the cement.

Comparative example No. three

The cement grinding aid comprises the following components in parts by weight: 200 parts of tobacco stem black liquor, 20 parts of sulfonating agent, 120 parts of waste molasses, 100 parts of triethanolamine, 100 parts of sodium lignosulfonate, 50 parts of thickening agent, 80 parts of sodium sulfate solution and 200 parts of water.

Wherein, the thickening agent is one or more of hydroxypropyl methylcellulose and hydroxyethyl cellulose, and the sulfonating agent is one or more of ammonium bisulfite, sulfuric acid and sodium sulfite.

In the comparative example, a preparation method of the cement grinding aid is also provided, and the preparation method comprises the following steps:

s1: taking the tobacco stalk black liquor, and adjusting the pH value of the tobacco stalk black liquor to 10 by using a sodium hydroxide or hydrochloric acid solution for later use;

s2: adding the sulfonating agent into the treatment solution of S1, carrying out continuous reaction at 80 ℃, carrying out continuous reaction for 240min, then carrying out spray drying, wherein the temperature of an atomizer of the spray drying equipment is 300 ℃, and the temperature of a spray outlet is 90 ℃, so as to obtain tobacco stem black liquor powder, and placing for later use;

s3: adding half of the water into a mixing kettle, then adding the waste molasses and the triethanolamine according to a proportion, and continuously stirring until the mixture is uniform to obtain a solution A;

s4: adjusting the temperature of the mixing kettle to 40 ℃, adding the tobacco stem black liquor powder in the S2 into the mixing kettle, and continuously stirring for 20min to obtain a solution B;

s5: adding sodium lignosulfonate and sodium sulfate solution into the other half of the water in a reaction kettle, sealing the reaction kettle, carrying out condensation reaction at 110 ℃, controlling the pressure at 2.0MPa for 8 hours, and cooling to room temperature to obtain solution C;

s6: adding the solution C into the solution B, stirring while adding, and keeping the temperature at 50 ℃ until the solution is uniform to obtain a solution E;

s7: and adding a thickening agent into the solution E, keeping the temperature at 40 ℃, and stirring for 20min until the solution is uniform to obtain the finished cement grinding aid.

Specifically, the method also comprises a using method of the cement grinding aid, wherein the cement grinding aid is directly used in the cement grinding process according to 0.03-0.05 percent of the total mass of the cement.

The cement grinding aids prepared in the first to fourth examples and the first to third comparative examples are tested, and the results are shown in the following table 1:

TABLE 1

The cement grinding aids prepared in the first to fourth examples and the first to third comparative examples were added to cement to prepare concrete, 500 g of each cement powder obtained in each example was taken, an equal amount of water was added to prepare concrete slabs having the same size and a thickness of 2cm, impact pressure was gradually increased to the surface thereof, and the pressure applied when the concrete broke was observed as shown in table 2:

TABLE 2

Crushing pressure
Example one 1280N
Example two 1315N
EXAMPLE III 1320N
Example four 1335N
Comparative example 1 1130N
Comparative example No. two 936N
Comparative example No. three 875N

According to the tables 1 and 2, in the first to fourth embodiments, after the cement grinding aid is added into the cement, under the same conditions, the yield of the mill is higher, the yield is kept between 28 t/h and 30t/h, the average particle size of the obtained cement particles is between 75 μm and 80 μm, the cement particles belong to smaller particles, and the efficiency and the quality of the mill powder are effectively improved; meanwhile, after the cement grinding aid in the first to fourth embodiments is used for preparing concrete slabs which are identical in size and 2cm thick, the concrete can bear crushing pressure of 1250-1350N, the bearing capacity is good, and the compression resistance of the concrete can be effectively improved.

In the fourth embodiment and the first comparative example which are all the same under other conditions, after the pretreatment of the black liquid of the tobacco stalk is carried out, in the mixing treatment process of the black liquid, waste molasses and triethanolamine, flavone is not added for auxiliary treatment, so that the cement grinding aid obtained in the first comparative example has the advantages that under the same conditions, the yield of a mill is general and is only 20.72t/h, meanwhile, the average particle size of the obtained cement particles is also larger, the efficiency of mill powder is general, and the quality is general;

in the fourth embodiment and the second comparative example, the second comparative example does not carry out limonin treatment on the mixed solution of sodium lignosulfonate and sodium sulfate solution, but directly mixes with the solution B, and the obtained cement grinding aid only bears 936N in the concrete compression resistance test, so that the compression resistance of the concrete prepared by the aid of the cement grinding aid is general;

in the fourth example and the third comparative example, in the mixing treatment process of the waste molasses and the triethanolamine, no flavone is added for auxiliary treatment, and no limonin treatment of the mixed solution of sodium lignosulfonate and sodium sulfate solution is carried out, so that after the cement grinding aid is applied, the yield of a mill is general, the average particle size of the obtained cement particles is large, and the compression resistance of concrete in a concrete compression resistance test is poor.

In conclusion, in the process of uniformly mixing the waste molasses, the triethanolamine and the black liquid of the tobacco stalks, the treatment liquid is obtained by adding the flavone for pretreatment, so that the mutual attraction of uniformly mixed substances is increased, the subsequent uniform mixing effect is promoted, the obtained cement grinding aid has good quality, the grinding efficiency and quality of a grinding machine can be effectively improved, the preparation treatment is carried out at graded temperature, the uniform mixing efficiency of each substance is high, the limonin is added at the regulated temperature, and the compressive capacity of the finished concrete can be greatly improved in the process of applying the finally obtained cement grinding aid.

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.

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