CN112174566B - Preparation method of powder modified protein gypsum retarder - Google Patents
Preparation method of powder modified protein gypsum retarder Download PDFInfo
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- CN112174566B CN112174566B CN202011044973.7A CN202011044973A CN112174566B CN 112174566 B CN112174566 B CN 112174566B CN 202011044973 A CN202011044973 A CN 202011044973A CN 112174566 B CN112174566 B CN 112174566B
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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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/003—Phosphorus-containing compounds
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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
- C04B40/0042—Powdery mixtures
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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
- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
-
- 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
- C04B2103/20—Retarders
- C04B2103/22—Set retarders
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention relates to the field of building materials, in particular to a preparation method of a powder modified protein gypsum retarder for a gypsum building material. The powder modified protein gypsum retarder prepared by the invention has high content of effective protein components and good retarding effect, can obviously delay the setting time of gypsum due to low doping amount, and has better retarding effect in neutral and alkaline environments; the self-leveling gypsum plaster can be widely used for gypsum self-leveling, plastering gypsum and other dry powder gypsum products, the interval between the initial setting time and the final setting time is effectively prolonged, and the concentrated heating in the gypsum hardening process is reduced; the preparation method of the powder modified protein gypsum retarder has the advantages that no waste water, waste gas and solid waste are generated in the whole process, and the whole process flow can be operated in a flow mode.
Description
Technical Field
The invention relates to the field of building materials, in particular to a preparation method of a powder modified protein gypsum retarder for a gypsum building material.
Background
The gypsum is a green building material with excellent performance and recycling, the natural gypsum storage amount of China is at the top of the world, the comprehensive utilization rate of industrial byproducts is low, the accumulated quantity of the industrial byproduct gypsum exceeds 3 hundred million tons, and the gypsum can be widely applied to products such as plastering gypsum, self-leveling gypsum, gypsum boards, GRC gypsum components and the like. The gypsum is set and hardened quickly and can be used after the operation time is prolonged, and the gypsum retarder is an indispensable component in the gypsum building material.
The gypsum retarder is mainly divided into organic acid and soluble salt thereof, alkaline phosphate and protein, the organic acid and soluble salt thereof mainly comprise citric acid, sodium citrate, tartaric acid, potassium tartrate and the like, wherein the best effect is citric acid and salt thereof, but the strength of the building gypsum is obviously reduced, and the larger the mixing amount is, the more obvious the strength reduction is. Phosphate retarders mainly comprise sodium hexametaphosphate, sodium polyphosphate, sodium tripolyphosphate, sodium pyrophosphate and the like, but the retarder has low retarding efficiency, high mixing amount and large influence on strength. The protein retarder comprises bone glue, peptone and the like, has relatively small influence on the crystal morphology of the dihydrate gypsum, has small strength loss, but has higher cost, short initial and final setting time interval and poor retarding effect in an alkaline environment.
The patent with publication number CN 106495517A discloses a method for utilizing livestock and poultry slaughter waste, which takes the livestock and poultry slaughter waste as a raw material, prepares a gypsum retarder through the steps of physical purification, acid hydrolysis, trisodium phosphate modification and the like, and obtains an acid hydrolysis liquid protein gypsum retarder, wherein the initial and final setting time interval of the gypsum retarder is short, and the retarding effect of an alkaline environment is not reflected.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: in order to overcome the defects in the prior art, a preparation method of a powder modified protein gypsum retarder is provided.
The technical scheme adopted by the invention is as follows: a preparation method of a powder modified protein gypsum retarder comprises the following steps:
a. acid hydrolysis: putting 30-35 parts by mass of protein raw material, 10-18 parts by mass of 31% hydrochloric acid and 40-45 parts by mass of water into a reactor, and performing hydrolysis reaction for 3-4h at the temperature of 85-90 ℃ to obtain acidolysis protein solution with the solid content of 35-40%;
b. modification: b, leaving 60-70 parts by mass of the acidolysis protein solution obtained in the step a in a reactor, adding 25-35 parts by mass of organic phosphonic acid, 1-2 parts by mass of styrene sulfonic acid and 4-8 parts by mass of hydroxyethyl acrylate, and keeping the mixture at the temperature of 55-60 ℃ for 1-1.5 hours to obtain a mixture;
c. neutralizing: cooling the mixture obtained in the step b to 35-45 ℃, adding 3-6 parts by mass of potassium tartrate and 5-15 parts by mass of alkali substances, and neutralizing the pH value to 7-9 to obtain a modified opal retarder solution;
d. adsorption: c, mixing the modified protein gypsum retarder solution obtained in the step c and perlite according to a mass ratio of 5-6: 1, mixing and stirring to ensure that the coagulant solution is fully adsorbed on the perlite to obtain perlite for adsorbing solution;
e. drying: d, passing the perlite adsorbing the solution obtained in the step d through a drying channel, setting the temperature to be 160-200 ℃, and drying until the moisture content is below 5% to obtain perlite particles;
f. grinding: and e, grinding the perlite particles obtained in the step e to powder with more than 100 meshes by using grinding equipment to form the powder modified protein gypsum retarder.
The protein raw material in the step a is waste such as poultry feather, cattle and sheep subcutaneous leftovers and the like.
The organic phosphonic acid in the step b is one, two or three of diethylenetriamine pentamethylene phosphonic acid, hexamethylene diamine tetramethylidene phosphonic acid and hydroxyl phosphono acetic acid.
And the alkali substance in the step c is one, two or three of calcium hydroxide, magnesium hydroxide and aluminum hydroxide.
Organic phosphonic acid, styrene sulfonic acid and hydroxyethyl acrylate are added into the acidolysis protein solution, phosphonic acid groups, acrylic acid groups and sulfonic acid groups with chelating capacity for calcium ions are introduced, the phosphonic acid groups, the acrylic acid groups and the sulfonic acid groups have a composite action with the acidolysis protein, the calcium tolerance is improved, and the obtained retarder has a good retarding effect in neutral and alkaline environments.
Compared with the prior art, the invention has the following advantages:
1. the powder modified opal retarder prepared by the invention has high content of effective protein components, good retarding effect, low doping amount, good retarding effect in neutral and alkaline environments and capability of obviously delaying the setting time of gypsum;
2. the powder modified opal retarder prepared by the invention can be widely used for dry powder gypsum products such as gypsum self-leveling gypsum, plastering gypsum and the like, the interval between the initial setting time and the final setting time is effectively prolonged, and the concentrated heating in the gypsum hardening process is reduced;
3. the preparation method of the powder modified protein gypsum retarder has the advantages that no waste water, waste gas and solid waste are generated in the whole process, and the whole process flow can be operated in a flow mode.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the embodiments of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
A preparation method of a powder modified protein gypsum retarder comprises the following steps:
a. acid hydrolysis: putting 30 parts by mass of protein raw material, 10 parts by mass of 31% hydrochloric acid and 40 parts by mass of water into a reactor, and performing hydrolysis reaction for 3-4h at the temperature of 85-90 ℃ to obtain acidolysis protein solution with the solid content of 35-40%;
b. modification: leaving 60 parts by mass of the acidolysis protein solution obtained in the step a in a reactor, adding 25 parts by mass of diethylenetriamine pentamethylenephosphonic acid, 1 part by mass of styrene sulfonic acid and 4 parts by mass of hydroxyethyl acrylate, and keeping the mixture at the temperature of 55-60 ℃ for 1-1.5 hours to obtain a mixture;
c. neutralizing: cooling the mixture obtained in the step b to 35-45 ℃, and then adding 3 parts by mass of potassium tartrate and 5 parts by mass of calcium hydroxide, wherein the pH value of neutralization is 7-9, so as to obtain a modified opal retarder solution;
d. adsorption: and d, mixing the modified protein gypsum retarder solution obtained in the step c and perlite according to a mass ratio of 5: 1, mixing and stirring to ensure that the coagulant solution is fully adsorbed on the perlite to obtain perlite for adsorbing solution;
e. drying: d, passing the perlite adsorbing the solution obtained in the step d through a drying channel, setting the temperature to be 160-200 ℃, and drying until the moisture content is below 5% to obtain perlite particles;
f. grinding: and e, grinding the perlite particles obtained in the step e to powder with more than 100 meshes by using grinding equipment to form the powder modified protein gypsum retarder.
Four parts of desulfurized semi-hydrated gypsum with the same specification are taken, wherein one part of desulfurized semi-hydrated gypsum is not added with a retarder, the other part of desulfurized semi-hydrated gypsum is added with peptone with the mass of 0.2 percent of that of the desulfurized semi-hydrated gypsum, the other part of desulfurized semi-hydrated gypsum is added with bone glue protein with the mass of 0.2 percent of that of the desulfurized semi-hydrated gypsum, and the retarder prepared in the embodiment 1 with the mass of 0.2 percent of that of the desulfurized semi-hydrated gypsum is added, and then the performances of the desulfurized semi-hydrated gypsum are tested, and the results are as follows:
taking four parts of desulfurized semi-hydrated gypsum and ash calcium powder with the same specification according to the mass ratio of 20: 1, one part of the mixed gypsum is not added with a retarder, one part of the mixed gypsum is added with peptone of which the mass is 0.2 percent of that of the mixed gypsum, one part of the mixed gypsum is added with bone glue protein of which the mass is 0.2 percent of that of the mixed gypsum, and one part of the mixed gypsum is added with the retarder of which the mass is 0.2 percent of that of the mixed gypsum and prepared in the embodiment 1, and then the performances of the desulfurized semi-hydrated gypsum are tested, and the results are as follows:
example 2
A preparation method of a powder modified protein gypsum retarder comprises the following steps:
a. acid hydrolysis: putting 35 parts by mass of a protein raw material, 18 parts by mass of 31% hydrochloric acid and 45 parts by mass of water into a reactor, and performing hydrolysis reaction for 3-4 hours at the temperature of 85-90 ℃ to obtain an acidolysis protein solution with the solid content of 35-40%;
b. modification: leaving 60 parts by mass of the acidolysis protein solution obtained in the step a in a reactor, adding 25 parts by mass of diethylenetriamine pentamethylenephosphonic acid, 1 part by mass of styrene sulfonic acid and 4 parts by mass of hydroxyethyl acrylate, and keeping the mixture at the temperature of 55-60 ℃ for 1-1.5 hours to obtain a mixture;
c. neutralizing: cooling the mixture obtained in the step b to 35-45 ℃, and then adding 3 parts by mass of potassium tartrate and 5 parts by mass of calcium hydroxide, wherein the pH value of neutralization is 7-9, so as to obtain a modified opal retarder solution;
d. adsorption: and d, mixing the modified protein gypsum retarder solution obtained in the step c and perlite according to a mass ratio of 5: 1, mixing and stirring to ensure that the coagulant solution is fully adsorbed on the perlite to obtain perlite for adsorbing solution;
e. drying: d, passing the perlite adsorbing the solution obtained in the step d through a drying channel, setting the temperature to be 160-200 ℃, and drying until the moisture content is below 5% to obtain perlite particles;
f. grinding: and e, grinding the perlite particles obtained in the step e to powder with more than 100 meshes by using grinding equipment to form the powder modified protein gypsum retarder.
Taking four parts of phosphogypsum with the same specification, wherein one part of phosphogypsum is not added with a retarder, the other part of phosphogypsum is added with citric acid with the mass of 0.2 percent of the phosphogypsum, the other part of phosphogypsum is added with sodium hexametaphosphate with the mass of 0.2 percent of the phosphogypsum, and the other part of the retarder prepared in the embodiment 1 with the mass of 0.2 percent of the phosphogypsum is added with the phosphogypsum, and then testing the performances of the phosphogypsum is carried out, and the results are as follows:
the test results of the above examples 1, 2 and 3 show that the powder modified protein gypsum retarder prepared by the preparation method has small retardation time change in a neutral system and an alkaline system, has good retardation effect and wider adaptability when being added into desulfurized semi-hydrated gypsum and phosphogypsum, has the initial and final setting time difference of more than 30 minutes, can effectively reduce concentrated heating in the gypsum hardening process, provides constructors with longer operation time, and improves the surface treatment effect of gypsum products (gypsum self-leveling and gypsum putty).
Claims (3)
1. A preparation method of a powder modified protein gypsum retarder is characterized by comprising the following steps:
a. acid hydrolysis: putting 30-35 parts by mass of protein raw material, 10-18 parts by mass of 31% hydrochloric acid and 40-45 parts by mass of water into a reactor, and performing hydrolysis reaction for 3-4h at the temperature of 85-90 ℃ to obtain acidolysis protein solution with the solid content of 35-40%;
b. modification: b, leaving 60-70 parts by mass of the acidolysis protein solution obtained in the step a in a reactor, adding 25-35 parts by mass of organic phosphonic acid, 1-2 parts by mass of styrene sulfonic acid and 4-8 parts by mass of hydroxyethyl acrylate, and keeping the mixture at the temperature of 55-60 ℃ for 1-1.5 hours to obtain a mixture;
c. neutralizing: cooling the mixture obtained in the step b to 35-45 ℃, adding 3-6 parts by mass of potassium tartrate and 5-15 parts by mass of alkali substances, and neutralizing the pH value to 7-9 to obtain a modified opal retarder solution;
d. adsorption: c, mixing the modified protein gypsum retarder solution obtained in the step c and perlite according to a mass ratio of 5-6: 1, mixing and stirring to ensure that the coagulant solution is fully adsorbed on the perlite to obtain perlite for adsorbing solution;
e. drying: d, passing the perlite adsorbing the solution obtained in the step d through a drying channel, setting the temperature to be 160-200 ℃, and drying until the moisture content is below 5% to obtain perlite particles;
f. grinding: d, grinding the perlite particles obtained in the step e to powder with the particle size of more than 100 meshes through grinding equipment to form a powder modified opal retarder;
the organic phosphonic acid in the step b is one, two or three of diethylenetriamine pentamethylene phosphonic acid, hexamethylene diamine tetramethylidene phosphonic acid and hydroxyl phosphono acetic acid.
2. The method for preparing the powder modified protein gypsum retarder according to claim 1, which is characterized in that: the protein raw material in the step a is waste such as poultry feather, cattle and sheep subcutaneous leftovers and the like.
3. The method for preparing the powder modified protein gypsum retarder according to claim 1, which is characterized in that: and the alkali substance in the step c is one, two or three of calcium hydroxide, magnesium hydroxide and aluminum hydroxide.
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| CN115504702B (en) * | 2022-11-01 | 2023-07-28 | 邯郸市潘仁新能源科技有限公司 | Organic acid-protein composite gypsum retarder and preparation method thereof |
| CN115651113B (en) * | 2022-11-15 | 2023-09-01 | 江苏尼高科技有限公司 | Preparation process of gypsum retarder |
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| EP2274252A1 (en) * | 2008-04-10 | 2011-01-19 | Sika Technology AG | Setting retarder for hydraulically hardening compounds |
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