CN113998919B - Composite water reducing agent prepared from silicon-containing wastewater and preparation method and application thereof - Google Patents
Composite water reducing agent prepared from silicon-containing wastewater and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a composite water reducing agent prepared from silicon-containing wastewater, a preparation method and application thereof, wherein the preparation method comprises the following steps: (1) Uniformly mixing 60-90 parts by mass of silicon-containing wastewater, 0.2-4 parts by mass of phosphorous acid and/or hypophosphite, 1-15 parts by mass of water, 1-15 parts by mass of liquid alkali, 0.1-2 parts by mass of maleic anhydride and 1-10 parts by mass of acrylic acid, and heating to 50-90 ℃; (2) Then adding an initiator solution, and reacting for 1.5-3.5 h under heat preservation; (3) And then adding a chain transfer agent solution to terminate the reaction, and stopping heating to obtain the composite water reducing agent. The composite water reducing agent has good dispersibility, and avoids the difficult problems of flocculation and the like caused by uneven stirring of the polycarboxylic acid water reducing agent and water glass. Meanwhile, the composite water reducing agent has the advantages of low cost, simple process, environmental protection and high resource utilization rate, can effectively utilize waste byproducts, realizes changing waste into valuable, and has good economic and environmental benefits.
Description
Technical Field
The invention belongs to the technical field of ceramic industry and fine chemical industry, and particularly relates to a method for preparing a composite water reducing agent by using byproducts and application of the composite water reducing agent.
Background
The development of comprehensive utilization of resources is a long-term strategic policy in national economy and social development, and has important significance in relieving increasingly strengthened resource environmental constraints in the process of industrialization and urbanization, improving the utilization efficiency of resources and enhancing the sustainable development capability. Several thousand tons of methyl dichlorosilane and trimethyl chlorosilane are generated in the production of the organic silicon monomer every year, after the methyl dichlorosilane and the trimethyl chlorosilane are hydrolyzed, acidified and treated by alkali liquor, the silane obtained by partial hydrolysis is comprehensively utilized, and the silicone oil with economic benefit is prepared by reaction; the balance is silicon-containing wastewater containing one or more of silane mixture containing Si-Si, si-C-Si and Si-O-Si, aluminum silicate, calcium silicate, sodium silicate and sodium sulfate. Limited by environmental protection policies, these wastewaters are hazardous and cannot be dumped at will; moreover, disposal by the recycling companies increases the cost of the enterprise; more seriously, the normal production of enterprises is greatly influenced along with the accumulation of byproduct wastewater. If the production by-products are recycled and prepared into the novel water reducer, the waste water reducer is changed into treasure, and the novel water reducer has the advantage of low raw material cost and accords with the development of green chemistry. Not only improves the utilization efficiency of resources and reduces the cost of enterprises, but also reduces the pollution to the environment.
In patent CN202010937185.4, many high-efficiency water reducing agents with flexible long-chain structures are prepared, but the synthesis difficulty is high, and N is required for reaction 2 Protection; the chloroplatinic acid with high use cost is not beneficial to industrialization. In patent CN202110368092.9, a compound water reducing agent with good adaptability is prepared, but a small amount of naphthalene water reducing agent is used, which is not favorable for environmental protection. As the raw materials for producing the naphthalene-based superplasticizer comprise industrial naphthalene, sulfuric acid, formaldehyde and the like, the environment is polluted. Patent CN202010860267.3, prepared a compound water reducing agent based on polycarboxylic acid, the cost is lower, but because the water content is close to 80% due to the dilution with water, the dispersion effect is relatively reduced. Patent CN 201811506366.0 utilizes the complementation of sodium silicate and sodium polyacrylate to realize the dispergation effect of mud in each time period. But the peptization effect of the sodium polyacrylate and the sodium tripolyphosphate is greatly weakened after crystallization and solidification.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the invention aims to provide a method for preparing a composite water reducing agent by utilizing byproducts and application thereof.
The purpose of the invention is realized by the following technical scheme:
a method for preparing a composite water reducing agent by using silicon-containing wastewater comprises the following steps:
(1) Uniformly mixing 60-90 parts by mass of silicon-containing wastewater, 0.2-4 parts by mass of phosphorous acid and/or hypophosphite, 1-15 parts by mass of water, 1-15 parts by mass of liquid alkali, 0.1-2 parts by mass of maleic anhydride and 1-10 parts by mass of acrylic acid, and heating to 50-90 ℃;
(2) Then adding an initiator solution, and reacting for 1.5-3.5 h under heat preservation;
(3) And then adding a chain transfer agent solution to terminate the reaction, and stopping heating to obtain the composite water reducing agent.
Preferably, the silicon-containing wastewater accounts for 70-80 parts by mass, the phosphorous acid and/or the hypophosphite accounts for 0.5-2.5 parts by mass, the water accounts for 4-12 parts by mass, the liquid alkali accounts for 6-10 parts by mass, the maleic anhydride accounts for 0.5-1 part by mass, and the acrylic acid accounts for 1-6 parts by mass.
Preferably, the silicon-containing wastewater is organosilicon production wastewater, and the solid content of the wastewater is 30 +/-5%.
Preferably, the conditions of the incubation reaction are: the temperature is 70-80 ℃, the time is 1.5-2.5h, and the stirring is continued at 100-300 rpm.
Preferably, the initiator solution is added dropwise, and the dropwise adding time is the same as the heat preservation reaction time.
Preferably, the initiator is one or more than two of potassium permanganate, potassium dichromate, ammonium persulfate, potassium persulfate and sodium persulfate; the chain transfer agent is one or more than two of sodium polysulfide, phosphorous acid, sodium hypophosphite and sodium dimethyldithiocarbamate.
Preferably, the hypophosphite is sodium hypophosphite or potassium hypophosphite; the liquid alkali is sodium hydroxide solution or potassium hydroxide solution, and the mass concentration of the liquid alkali is 50 +/-10%; 0.1 to 1.5 parts by mass of initiator solution with the mass concentration of 4 +/-2 percent; the mass concentration of the chain transfer agent solution is 0.1-1.5 parts, and the mass concentration is 1 +/-0.5%; and the solvents of the initiator solution and the chain transfer agent solution are both water.
The viscosity of the composite water reducing agent prepared by the method is 100-400 cp (25 ℃,100 rpm), and is measured by a Brooks rotational viscometer, so that the viscosity is low.
The application field of the composite water reducing agent is architectural ceramics and sanitary ceramics, and the composite water reducing agent is used for slurry dispersion.
Conventional polymeric dispersants generally maintain the dispersing properties of the dispersed particles by two actions: (1) electric double layer action: the dispersing agent makes the dispersed particles have the same charge on the surface, and when the dispersed particles are contacted with each other, the dispersed particles repel each other due to the same charge, so that the charged particles maintain the stability of the system under the action of Coulomb repulsion force. (2) steric hindrance: the polymeric dispersant adsorbed on the surface of the dispersed particles acts as a mechanical barrier to the particles, making interparticle contact impossible, and the strong interaction between the polymeric dispersant and water prevents excessive access to the pigment particles.
The composite water reducing agent is an organic and inorganic composite system, good hydrophilic groups such as phosphorus and carboxylic acid are introduced, hydrophobic groups of a better flexible chain are designed, and under the synergistic effect of inorganic salt, the dispersibility and the stability are improved, and the composite water reducing agent has the advantages of high-efficiency dispersibility of an organic polymer dispersing agent and low cost of an inorganic dispersing agent.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) The composite water reducing agent disclosed by the invention utilizes organic silicon production wastewater as a raw material, is high in resource utilization rate, changes waste into valuable, and has good economic and environmental benefits.
(2) Compared with the traditional polycarboxylic acid and water glass compound water reducing agent system, the compound water reducing agent has obvious price advantage, the silicon-containing wastewater has extremely low cost, is freely provided by manufacturers, and only needs to spend transportation cost. Meanwhile, the water reducing agent has good dispersibility, and the difficult problems of flocculation and the like caused by uneven stirring of the polycarboxylate water reducing agent and water glass are avoided.
(3) Compared with a naphthalene water reducer and water glass compound system, the composite water reducer is simple to synthesize and environment-friendly.
(4) The composite water reducing agent disclosed by the invention is an organic-inorganic composite system and has the advantages of good comprehensive performance and high cost performance.
Drawings
FIG. 1 is an infrared spectrum of the composite water reducing agent of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
(1) Weighing 70g of organic silicon production wastewater (silane mixture containing Si-O-Si, aluminum silicate, calcium silicate, sodium sulfate and the like as components), 1g of phosphorous acid, 2g of sodium hypophosphite, 5g of water, 15g of sodium hydroxide solution with the mass concentration of 50%, 0.5g of maleic anhydride and 5g of acrylic acid, uniformly stirring, and heating to 80 ℃.
(2) 0.5g of a 4% strength by mass potassium permanganate solution was added, stirring was continued, and the reaction was carried out at 80 ℃ for 1.5h.
(3) And adding 1g of sodium polysulfide solution with the mass concentration of 1%, stopping heating, and continuously stirring for 30min to obtain the composite water reducing agent.
The testing method of the dispersibility of the composite water reducing agent comprises the following steps: 1.4g of the composite water reducing agent is dissolved in 112.5g of water, 200g of ball clay EC30 of Yingke ceramics materials Co., ltd, in Jiangmen, is added, and is ball-milled for 10min in a planet ball mill, and then zirconium balls are filtered and separated by a screen to obtain uniform slurry. The time for completing the slurry flow was measured 3 times using 4 cups, and the average value was found to be 24.4s, indicating good dispersion properties.
Example 2
(1) 75g of organosilicon production wastewater (same as in example 1), 0.5g of phosphorous acid, 0.5g of sodium hypophosphite, 12g of water, 4g of 50% sodium hydroxide solution, 1g of maleic anhydride and 6g of acrylic acid are weighed, stirred uniformly and heated to 75 ℃.
(2) 0.5g of a 4% strength by mass potassium dichromate solution was added, stirred continuously, and reacted at 75 ℃ for 2 hours.
(3) And adding 0.5g of sodium polysulfide solution with the mass concentration of 1%, stopping heating, and continuously stirring for 30min to obtain the composite water reducing agent.
The testing method of the dispersibility of the composite water reducing agent comprises the following steps: 1.4g of the composite water reducing agent is dissolved in 112.5g of water, 200g of ball clay EC30 of Yingke ceramic raw material Co., ltd, jiangmen is added, ball milling is carried out in a planet ball mill for 10min, and then zirconium balls are filtered and separated by a screen to obtain uniform slurry. The time for completing the slurry flow was measured 3 times using 4 cups, and the average value was found to be 25.1s, indicating good dispersibility.
Example 3
(1) 80g of organosilicon process wastewater (same as in example 1), 1.5g of phosphorous acid, 4.3g of water, 3g of 50% by mass potassium hydroxide solution, 0.2g of maleic anhydride and 10g of acrylic acid are weighed, stirred uniformly and heated to 75 ℃.
(2) 0.6g of a 4% strength by mass ammonium persulfate solution was added, stirred continuously, and reacted at 75 ℃ for 2.5 hours.
(3) And adding 0.4g of phosphorous acid solution with the mass concentration of 1%, stopping heating, and continuously stirring for 30min to obtain the composite water reducing agent.
The testing method of the dispersibility of the composite water reducing agent comprises the following steps: 1.4g of the composite water reducing agent is dissolved in 112.5g of water, 200g of ball clay EC30 of Yingke ceramics materials Co., ltd, in Jiangmen, is added, and is ball-milled for 10min in a planet ball mill, and then zirconium balls are filtered and separated by a screen to obtain uniform slurry. The time for completing the slurry flow was measured 3 times using 4 cups, and the average value was found to be 25.5s, indicating good dispersibility.
Example 4
(1) 85g of organosilicon production wastewater (same as in example 1), 2g of phosphorous acid, 0.5g of sodium hypophosphite, 5g of water, 2g of 50% by mass potassium hydroxide solution, 2g of maleic anhydride and 2g of acrylic acid are weighed, stirred uniformly and heated to 70 ℃.
(2) 1g of a 4% strength by mass potassium persulfate solution was added, stirred continuously and reacted at 70 ℃ for 3 hours.
(3) And adding 0.5g of sodium hypophosphite solution with the mass concentration of 1%, stopping heating, and continuously stirring for 30min to obtain the composite water reducing agent.
The testing method of the dispersibility of the composite water reducing agent comprises the following steps: 1.4g of the composite water reducing agent is dissolved in 112.5g of water, 200g of ball clay EC30 of Yingke ceramics materials Co., ltd, in Jiangmen, is added, and is ball-milled for 10min in a planet ball mill, and then zirconium balls are filtered and separated by a screen to obtain uniform slurry. The time for completing the slurry flow was measured 3 times using 4 cups, and the average value was found to be 26.7s, indicating good dispersion properties.
Example 5
(1) 90g of organosilicon production wastewater (same as in example 1), 0.5g of sodium hypophosphite, 6g of water, 1g of 50% sodium hydroxide solution, 0.8g of maleic anhydride and 1g of acrylic acid are weighed, stirred uniformly and heated to 70 ℃.
(2) 0.2g of a 4% strength by mass sodium persulfate solution was added, stirred continuously, and reacted at 70 ℃ for 3.5 hours.
(3) And adding 0.5g of a 1% sodium dimethyldithiocarbamate solution, stopping heating, and continuously stirring for 30min to obtain the composite water reducing agent.
The testing method of the dispersibility of the composite water reducing agent comprises the following steps: 1.4g of the composite water reducing agent is dissolved in 112.5g of water, 200g of ball clay EC30 of Yingke ceramics materials Co., ltd, in Jiangmen, is added, and is ball-milled for 10min in a planet ball mill, and then zirconium balls are filtered and separated by a screen to obtain uniform slurry. The time for which the slurry was discharged was measured 3 times using 4 cups, and the average value was found to be 31.3s, indicating that the dispersibility was good.
Comparative example 1
(1) 80g of organosilicon production wastewater (same as in example 1), 0.2g of phosphorous acid, 5.6g of water, 3g of 50% by mass potassium hydroxide solution, 0.2g of maleic anhydride and 10g of acrylic acid are weighed, stirred uniformly and heated to 75 ℃.
(2) 0.6g of a 4% strength by mass ammonium persulfate solution was added, stirred continuously, and reacted at 75 ℃ for 2.5 hours.
(3) And adding 0.4g of phosphorous acid solution with the mass concentration of 1%, stopping heating, and continuously stirring for 30min to obtain the composite water reducing agent.
The testing method of the dispersibility of the composite water reducing agent comprises the following steps: 1.4g of the composite water reducing agent is dissolved in 112.5g of water, 200g of ball clay EC30 of Yingke ceramic raw material Co., ltd, jiangmen is added, ball milling is carried out in a planet ball mill for 10min, and then zirconium balls are filtered and separated by a screen to obtain uniform slurry. The time for completing the slurry flow was measured 3 times using 4 cups, and the average value was found to be 47.2s. The fluidity was inferior to that of example 3.
Comparative example 2
(1) 90g of organosilicon production wastewater (same as in example 1), 0.4g of sodium hypophosphite, 6.1g of water, 1g of 50% sodium hydroxide solution, 0.8g of maleic anhydride and 1g of acrylic acid are weighed, stirred uniformly and heated to 70 ℃.
(2) 0.2g of a 4% strength by mass sodium persulfate solution was added, stirred continuously, and reacted at 70 ℃ for 3.5 hours.
(3) And adding 0.5g of a 1% sodium dimethyldithiocarbamate solution, stopping heating, and continuously stirring for 30min to obtain the composite water reducing agent.
The method for testing the dispersibility of the composite water reducing agent comprises the following steps: 1.4g of the composite water reducing agent is dissolved in 112.5g of water, 200g of ball clay EC30 of Yingke ceramic raw material Co., ltd, jiangmen is added, ball milling is carried out in a planet ball mill for 10min, and then zirconium balls are filtered and separated by a screen to obtain uniform slurry. The time for completing the slurry flow was measured 3 times using 4 cups and the average value was found to be 36.4s. Compared with example 5, the phosphorus-containing hydrophilic group is reduced, and the dispersibility is weakened; and the content of the chain transfer agent is lower, so that the molecular weight and the molecular weight distribution of the water reducing agent are influenced. Finally, the viscosity of the slurry is increased, the flowing time is increased, and the fluidity is deteriorated.
Comparative example 3
0.9g of a high efficiency ceramic water reducing agent CA100 of Guangzhou chemical company, guangzhou, china, is dissolved in 112.5g of water, 200g of ball clay EC30 of Yikelong ceramic raw material company, china, is added, ball milling is carried out in a planetary ball mill for 10min, and then zirconium balls are filtered and separated by a screen to obtain uniform slurry. The time for completing the slurry flow was measured 3 times using 4 cups, and the average value was found to be 12.9s, indicating that the dispersion property was good. However, the cost of CA100 is 8 times of that of the composite water reducing agent of the invention. After conversion, the invention has cost advantage.
Comparative example 4
0.8g of a high efficiency ceramic water reducing agent CA100 of Guangzhou chemical company, guangzhou, china, was dissolved in 112.5g of water, 200g of ball clay EC30 of Yikelong ceramic raw material company, china, etc. was added, ball milling was performed in a planetary ball mill for 10min, and then zirconium balls were separated by filtering with a screen, but the slurry was thixotropic and viscous. The viscosity is too high to be applied to actual production. The performance of the water reducing agent is shown in the following table 1:
TABLE 1
The fluidity of the slurry can be measured by coating 4 cups to reflect the viscosity, the fluidity is good when the fluidity is less than 35s, the fluidity is general when the fluidity is 35-50 s, and the fluidity is weak when the fluidity is more than 60 s.
Thixotropy is expressed as the ratio of the flow time measured by standing for 30min to the initial mud flow time.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such modifications are intended to be included in the scope of the present invention.
Claims (10)
1. A method for preparing a composite water reducing agent by using silicon-containing wastewater is characterized by comprising the following steps:
(1) Uniformly mixing 60-90 parts by mass of silicon-containing wastewater, 0.5-4 parts by mass of phosphorous acid and/or hypophosphite, 1-15 parts by mass of water, 1-15 parts by mass of liquid alkali, 0.1-2 parts by mass of maleic anhydride and 1-10 parts by mass of acrylic acid, and heating to 50-90 ℃;
(2) Then adding an initiator solution, and reacting for 1.5-3.5 h under the condition of heat preservation;
(3) Then adding a chain transfer agent solution to terminate the reaction, and stopping heating to obtain the composite water reducing agent;
the silicon-containing wastewater is organic silicon production wastewater.
2. The method according to claim 1, wherein the silicon-containing wastewater is 70 to 80 parts by mass, the phosphorous acid and/or hypophosphite is 0.5 to 2.5 parts by mass, the water is 4 to 12 parts by mass, the liquid alkali is 6 to 10 parts by mass, the maleic anhydride is 0.5 to 1 part by mass, and the acrylic acid is 1 to 6 parts by mass.
3. The method as claimed in claim 1, wherein the silicon-containing wastewater has a solid content of 30 ± 5%.
4. The method according to claim 1, wherein the incubation reaction conditions are: the temperature is 70-80 ℃, the time is 1.5-2.5h, and the stirring is continued at 100-300 rpm.
5. The method of claim 1, wherein the initiator solution is added dropwise for the same time as the incubation reaction.
6. The method of claim 1, wherein the initiator is one or more of potassium permanganate, potassium dichromate, ammonium persulfate, potassium persulfate, and sodium persulfate; the chain transfer agent is one or more than two of sodium polysulfide, phosphorous acid, sodium hypophosphite and sodium dimethyldithiocarbamate.
7. The process according to any one of claims 1 to 6, wherein the hypophosphite is sodium hypophosphite or potassium hypophosphite; the liquid alkali is sodium hydroxide solution or potassium hydroxide solution, and the mass concentration of the liquid alkali is 50 +/-10%; 0.1 to 1.5 parts by mass of initiator solution with the mass concentration of 4 +/-2 percent; the mass of the chain transfer agent solution is 0.1-1.5 parts, and the mass concentration is 1 +/-0.5%; and the solvents of the initiator solution and the chain transfer agent solution are both water.
8. The composite water reducer prepared by the method of any one of claims 1 to 7.
9. The compound water reducer of claim 8, characterized in that the viscosity of the compound water reducer is 100-400 cp.
10. The use of the compound water reducer according to claim 8 or 9, characterized in that the compound water reducer is used for preparing building ceramics and sanitary ceramics.
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