CN111270312B - Method for preparing gypsum whisker from titanium gypsum - Google Patents
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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Abstract
The invention discloses a method for preparing gypsum whiskers by titanium gypsum, which comprises the following steps: 1) pretreating titanium gypsum to prepare powder, drying blocky titanium gypsum for 24 hours at 105 ℃, cooling and then grinding for 30min to prepare powder, and covering a plastic film in the air for aging for more than 7 days; 2) a decoloring treatment process, namely adding a proper amount of pretreated titanium gypsum powder into concentrated hydrochloric acid for dissolving, adding shell slaked lime for adjusting the pH value to 7, and filtering to form clear liquid and filter residue; putting the filter residue product into a vacuum drying oven, and drying at 200 ℃ to constant weight; 3) adding sodium sulfate, triethanolamine and glycerol as crystal modifier into the clear liquid, stirring and dissolving; pouring the obtained solution into a glass bottle, sealing and screwing a cover, putting the glass bottle into a vacuum drying oven, setting the temperature to 160 ℃, and heating for 4 hours; and opening after the reaction is completely cooled, performing suction filtration on a circulating water type multipurpose vacuum pump, and finally drying in a vacuum drying oven at 45 ℃ for 24 hours. The invention has the advantages of green and clean production process design and low cost.
Description
Technical Field
The invention belongs to the field of gypsum whisker preparation, and particularly relates to a method for preparing gypsum whiskers from titanium gypsum.
Background
The gypsum whisker is also called calcium sulfate whisker, is a fibrous crystal and has wide application prospect in the fields of building materials, chemical industry, environmental protection and the like. The composite material has the effects of high tensile strength, high toughness, fire resistance, flame retardance, wear resistance and chemical corrosion resistance, and the diameter is generally 0.1-8 mu m and the length is 0-300 mu m. Therefore, the gypsum whisker is suitable for being used as an ideal additive of cement-based materials as an environment-friendly, nontoxic and low-cost fiber reinforced material.
The quantity of industrial by-product gypsum in China is very large, and when titanium dioxide is produced by adopting a sulfuric acid method, lime (or carbide slag) is added to treat acid wastewater so as to neutralize a large amount of acid wastewater, so that C is producedaSO4·2H2O is industrial waste residue as main component. With the increasing demand of coatings and plastics, the titanium dioxide industry has a steadily increasing trend. 6-10 tons of titanium gypsum can be produced per 1 ton of titanium dioxide, the comprehensive utilization rate is about 10 percent, and the titanium gypsum is the byproduct gypsum with the lowest utilization rate. The large amount of emission not only occupies land, pollutes environment and destroys ecological balance, but also brings huge economic burden to titanium white enterprises and influences on expanded reproduction. The main methods for preparing the gypsum whisker by using the titanium gypsum comprise a normal-pressure salt method, a hydrothermal method, an organic solvent method and the like, and have excessive equipment and technical problems. The gypsum whisker has small yield, high price and little market demand. The industrialization of the gypsum whisker needs to solve the key preparation technology, reduce the cost and develop the market application. One of the technical difficulties in preparing white gypsum whiskers from titanium gypsum is poor whisker quality and low whiteness; secondly, the decoloring and purifying treatment leads the process to be complicated and the cost to be increased; thirdly, the traditional hydrothermal reaction preparation process needs corrosion-resistant equipment, and has long production period, unsafety and high cost; fourthly, the secondary pollution is caused by improper disposal of the waste water and the waste residue. Because no ideal comprehensive utilization technology causes a large amount of accumulation, the method has practical significance for scientific and efficient technical treatment.
Disclosure of Invention
The invention aims to provide a green process for preparing gypsum whiskers by titanium gypsum, and a process flow for preparing the gypsum whiskers by the titanium gypsum is designed, so that the key preparation technology is solved, the industrialization is achieved, and the application field of whisker materials is expanded. The glass material is used as a hydrothermal reaction container, and the method has the advantages of mild reaction, simple and convenient process, light weight, corrosion resistance and low cost. The water requirement is reduced and the whiteness of the whiskers is improved through pretreatment and decoloration processes. The sodium sulfate crystal-transformation agent is adopted to replace concentrated sulfuric acid in the traditional process, so that the growth of crystal whiskers is good, the quality is improved, and the corrosion of working procedures and equipment is reduced. The grinding-aid performance of the filtrate and the pigment and filler of the filter residue are functionally utilized, and a sustainable development gypsum whisker application industrial chain which is green, environment-friendly, low in cost and high in added value is created.
The scheme of the invention is as follows: a method for preparing gypsum whiskers by titanium gypsum comprises the following steps: drying the blocky titanium gypsum at 105 ℃ for 24h, grinding for 30min, covering the ground titanium gypsum with a preservative film, and aging for more than 7 d. Otherwise, efflorescence phenomenon and water demand increase easily occur, and the whiteness of the whisker and the production period are influenced.
And (3) a decoloring treatment process: adding ionized water into the pretreated titanium gypsum powder, and magnetically stirring and dispersing. Adding concentrated hydrochloric acid for dissolving, neutralizing with shell slaked lime, and filtering to obtain clear liquid and filter residue. And putting the filter residue product into a vacuum drying oven, and drying at the temperature of 200 ℃ until the weight is constant. The preparation of the shell slaked lime selects oyster shell with low iron content and high whiteness to calcine at 900 ℃, and keeps the temperature for 2 h. Cooling, taking out, placing in air, and automatically pulverizing to obtain white powder. Oyster shell need not to grind, and low price, the waste of utilizing is environmental protection.
The preparation process of the whisker comprises the following steps: adding sodium sulfate, triethanolamine and glycerol as crystal modifier into the clear liquid, stirring and dissolving completely. The resulting solution was poured into a 500ml glass bottle, the lid was sealed and tightened and placed in a vacuum oven, the temperature was set at 160 ℃ and heated for 4 h. And opening the reactor after the reaction is completely cooled, performing suction filtration on an SHB-IIIA circulating water type multipurpose vacuum pump, and finally drying the reactor in a vacuum drying oven at 45 ℃ for 24 hours. The prepared gypsum whisker has large length-diameter ratio, good dispersibility and 98 percent of whiteness. The conventional concentrated sulfuric acid crystal transfer agent is adopted, the crystal whisker is short and small, the agglomeration effect is obvious, a plurality of dendritic crystals are arranged, the disorder dispersibility is poor, and the length is uneven. The order of adding concentrated sulfuric acid is to add a crystal transformation procedure after the hydrothermal synthesis reaction is finished. Sodium sulfate is used as a crystal transformation agent instead of concentrated sulfuric acid, and the hydrothermal synthesis reaction and the crystal transformation are carried out integrally. Good growing of crystal whisker, easy dispersion, reduced acid pollution, simple process and low cost, and is beneficial to the subsequent application of waste liquid.
The invention discloses a green process for preparing gypsum whiskers by titanium gypsum, which comprises a powder preparation process by titanium gypsum pretreatment, a decoloring process and a whisker preparation process. Firstly, drying blocky titanium gypsum for 24 hours at 105 ℃, cooling and then grinding for 30min to prepare powder, and covering a plastic film in the air for aging for more than 7 d. Secondly, adding a proper amount of pretreated titanium gypsum powder into concentrated hydrochloric acid for dissolving, adding shell hydrated lime for adjusting the pH value to 7, and filtering to form clear liquid and filter residue. Thirdly, adding sodium sulfate, triethanolamine and glycerol as crystal-transforming agents into the clear liquid, fully dissolving and pouring into a glass bottle, wherein the content of the glass bottle is not more than 80 percent of the volume, and sealing the glass bottle with a cover. Heating at 160 ℃ for 4h, cooling, filtering the product, and drying in a vacuum drying oven at 45 ℃ for 24h to obtain white gypsum whisker with the whiteness of 98%. The process for preparing the red gypsum whisker does not comprise a decoloring process. The invention has the advantages that:
the green and clean production process design for preparing the gypsum whisker from the titanium gypsum realizes an industrial chain of green environmental protection, low cost and high added value and sustainable development.
Drawings
FIG. 1 is an XRD pattern of gypsum whisker and filter residue;
FIG. 2 is a sample of gypsum whiskers;
fig. 3 is a metallographic microscope photograph of a whisker-shaped gypsum crystal.
Detailed Description
The following examples are provided to illustrate the present invention.
Embodiment 1 a method for preparing gypsum whisker from titanium gypsum, comprising the following steps:
step 1: 1kg of blocky titanium gypsum is taken and dried for 24h at 95 ℃, is cooled and then is ground in a ball mill for 30min, the fineness is controlled to be less than 3.2 percent of the screen residue of a square-hole sieve with the fineness of 80 mu m, and the powder is covered with a preservative film and is aged for 7 d;
step 2: 5g of the pretreated titanium gypsum powder was weighed and dissolved in a 250ml beaker by adding 100ml of deionized water and magnetically stirring. Adding 7ml of concentrated hydrochloric acid, stirring for 2min to fully dissolve the agglomerated titanium gypsum, and standing for 5min after stirring;
and step 3: 500g of oyster shell is taken, cleaned and desanded, calcined at high temperature of 900 ℃ and kept at the constant temperature for 2 hours. Naturally cooling, taking out, stacking at room temperature, and automatically pulverizing into white powder.
And 4, step 4: adding shell slaked lime to adjust the pH value to 7, standing for 5min to allow undissolved titanium gypsum to naturally precipitate, and obviously observing solid-liquid delamination at the moment. Filtering the layered clear liquid on a funnel, putting filter residues into a vacuum drying oven, and setting the temperature to be 200 ℃ to constant weight;
and 5: sodium sulfate (3 g), triethanolamine (4 ml) and glycerol (4 ml) were added to the filtered clear solution, and sufficiently dissolved by stirring. The resulting solution was poured into a 500ml glass bottle with a volume of not more than 80%, and sealed with a cap. The glass bottle was placed in a vacuum drying oven, set to 140 ℃ and heated for 4 h. And after heating is finished, opening the reactor after the reaction is completely cooled, performing suction filtration on an SHB-IIIA circulating water type multipurpose vacuum pump, and finally drying the reactor in a vacuum drying oven at 45 ℃ for 24 hours to obtain the white gypsum whisker.
Embodiment 2 a method for preparing gypsum whisker from titanium gypsum, comprising the following steps:
step 1: drying 1kg of blocky titanium gypsum at 105 ℃ for 24h, cooling, and grinding in a ball mill for 30min, wherein the fineness is controlled to be less than 3.2% of the residue of a square-hole sieve with the fineness of 80 mu m, covering the powder with a preservative film, and aging for 8 d;
step 2: 6g of the pretreated titanium gypsum powder was weighed and dissolved in a 250ml beaker by adding 100ml of deionized water and magnetically stirring. Adding 8ml of concentrated hydrochloric acid, stirring for 2min to fully dissolve the agglomerated titanium gypsum, and standing for 5min after stirring;
and step 3: 500g of oyster shell is taken, cleaned and desanded, calcined at high temperature of 900 ℃ and kept at the constant temperature for 2 hours. Naturally cooling, taking out and stacking at room temperature. After absorbing water, the mixture becomes white powder;
and 4, step 4: adding shell slaked lime to adjust the pH value to 7, standing for 5 minutes to allow undissolved titanium gypsum to naturally precipitate, and obviously observing solid-liquid separation. Filtering the layered clear liquid on a funnel, putting filter residues into a vacuum drying oven, and setting the temperature to be 200 ℃ to constant weight;
and 5: sodium sulfate (3 g), triethanolamine (3 ml) and glycerol (5 ml) were added to the filtered clear solution, and sufficiently dissolved by stirring. The resulting solution was poured into a 500ml glass bottle with a volume of not more than 80%, and sealed with a cap. The glass bottle was placed in a vacuum drying oven, the temperature was set to 160 ℃ and heated for 4 h. And after heating is finished, opening the reactor after the reaction is completely cooled, performing suction filtration on an SHB-IIIA circulating water type multipurpose vacuum pump, and finally drying the reactor in a vacuum drying oven at 45 ℃ for 24 hours to obtain the white gypsum whisker.
Embodiment 3 a method for preparing gypsum whiskers from titanium gypsum, comprising the following steps:
step 1: drying 1kg of blocky titanium gypsum at 105 ℃ for 2h, cooling, and grinding in a ball mill for 30min, wherein the fineness is controlled to be less than 3.2% of the residue of a square-hole sieve with the fineness of 80 mu m, covering the powder with a preservative film, and aging for 8 d;
step 2: weighing 4g of pretreated gypsum powder, adding 100ml of deionized water and 8ml of glycerol, and magnetically stirring and dispersing. Pouring into 500ml glass bottle with the volume not exceeding 80%, and sealing with cap. The glass bottle was placed in a vacuum drying oven, the temperature was set at 150 ℃ and heated for 4 h. And after heating, opening the glass bottle after the glass bottle is completely cooled, performing suction filtration on an SHB-IIIA circulating water type multipurpose vacuum pump, and finally drying in a vacuum drying oven at 45 ℃ for 24 hours to obtain the mixture of impurities and gypsum whiskers.
Test examples
1. Raw materials:
shell: the shell is obtained from seafood processing shop, is oyster shell, and has high calcium content and good whiteness.
Shell slaked lime: cleaning oyster shell, calcining at 900 deg.C in high temperature furnace, and maintaining the temperature for 2 hr. Naturally cooling, taking out and stacking at room temperature. After absorbing water, the mixture became white powder.
Glycerol: analytically pure, Tianjin Bodi chemical Co., Ltd.
Triethanolamine: analytically pure, Tianjin Bodi chemical Co., Ltd.
Sodium sulfate: analytical purity, Henjin chemical reagents manufacturing Co., Ltd.
Concentrated hydrochloric acid: analytically pure, Tianjin Bodi chemical Co., Ltd.
Titanium gypsum: the chemical compositions are shown in Table 1.
TABLE 1 chemical composition of raw materials%
2. The test method comprises the following steps:
2.1 the preparation method of the gypsum whisker comprises the following steps:
crushing 1kg of titanium gypsum by using a hammer, drying in a drying oven at 105 ℃ and preserving heat for 24h, cooling and then grinding in a ball mill for 30min, covering the ground powder with a preservative film and aging for more than 7 d.
The white gypsum whisker preparation process flow comprises the following steps:
the preparation process flow of the impurity mixed gypsum whisker comprises the following steps:
3. test and result analysis
3.1 Effect of stoving temperature and aging time on the Properties of pretreated titanium Gypsum powder
The middle of the fresh titanium gypsum block taken back by the factory presents blue-green color, and the water content is as high as 45%. Breaking with hammer, and air drying for a while to obtain yellow powder. The drying temperature is low, and the titanium gypsum is completely adhered to the ball body during grinding. The drying temperature is 105 ℃ selected to reduce the drying time and improve the grinding efficiency, and the heat is preserved for 24 hours.
And (4) analyzing results: the pretreated titanium gypsum powder needs to be coated with a film on the surface, otherwise, the titanium gypsum powder absorbs water and is agglomerated. The titanium gypsum without pretreatment has high water content, agglomeration and white crystal precipitation on the surface.
TABLE 2 influence of aging time on the performance of the titanium gypsum pre-treated powder
Table 2 shows that 3d of old wine is quickly solidified into blocks by adding water. Avoid caking, increase water demand, but influence follow-up operation, drying time is long, and filtrate and filter residue volume are big, and gypsum whisker conversion reduces. Therefore, the problems of quick setting and agglomeration and incapability of dispersion can not occur when the aging time is selected to be more than 7 d.
3.2 influence of the crystal modifier on the morphology of the gypsum whisker
FIG. 2 shows that the whiteness of the gypsum whiskers prepared by adopting the decoloring treatment process reaches 98%, and the gypsum whiskers prepared without decoloring treatment have red impurities and a small amount of white gypsum whiskers which are mixed.
As shown in figure 3, the crystal transformation agent controls the crystal form of gypsum crystal development, and the length-diameter ratio is between 40 and 90. The concentrated sulfuric acid crystal-transformation agent is adopted, the crystal whisker is short and small, the agglomeration effect is obvious, a plurality of dendritic crystals are arranged, the disorder dispersibility is poor, and the length is not uniform. The order of adding concentrated sulfuric acid is to add a crystal transformation procedure after the hydrothermal synthesis reaction is finished. Sodium sulfate is used as a crystal transformation agent instead of concentrated sulfuric acid, and the hydrothermal synthesis reaction and the crystal transformation are carried out integrally. Good growing of crystal whisker, easy dispersion, reduced acid pollution, simple process and low cost, and is beneficial to the subsequent application of waste liquid.
Although specific embodiments of the invention have been described above, it will be understood by those skilled in the art that the specific embodiments of the invention described are illustrative only and are not limiting to the scope of the invention, and that equivalent modifications and variations can be made by those skilled in the art without departing from the spirit of the invention, which is to be covered by the appended claims.
Claims (4)
1. A method for preparing gypsum whiskers by titanium gypsum is characterized by comprising the following steps: the method comprises the following steps:
1) pretreating titanium gypsum to prepare powder, drying blocky titanium gypsum for 24 hours at 105 ℃, cooling and then grinding for 30min to prepare powder, and covering a plastic film in the air for aging for more than 7 days;
2) a decoloring treatment process, namely adding a proper amount of pretreated titanium gypsum powder into concentrated hydrochloric acid for dissolving, adding shell slaked lime for adjusting the pH value to 7, and filtering to form clear liquid and filter residue; putting the filter residue product into a vacuum drying oven, and drying at 200 ℃ to constant weight;
3) adding sodium sulfate, triethanolamine and glycerol as crystal modifier into the clear liquid, stirring and dissolving; pouring the obtained solution into a glass bottle, sealing and screwing a cover, putting the glass bottle into a vacuum drying oven, setting the temperature to 160 ℃, and heating for 4 hours; and opening after the reaction is completely cooled, performing suction filtration on a circulating water type multipurpose vacuum pump, and finally drying in a vacuum drying oven at 45 ℃ for 24 hours.
2. The method for preparing gypsum whiskers from titanium gypsum according to claim 1, wherein: in the step 2), oyster shells with low iron content and high whiteness are calcined at 900 ℃ and are kept warm for 2 hours; cooling, taking out, placing in air, and automatically pulverizing to obtain white powder.
3. The method for preparing gypsum whiskers from titanium gypsum according to claim 1, wherein: the weight parts of the raw materials are as follows: 4-6 parts of titanium gypsum pretreatment powder, 0-9 parts of concentrated hydrochloric acid, 0-3 parts of sodium sulfate, 0-7 parts of triethanolamine, 3-10 parts of glycerol and 0-18 parts of shell hydrated lime.
4. The method for preparing gypsum whiskers from titanium gypsum according to claim 3, wherein: 6 parts of pretreated titanium gypsum powder; 9 parts of hydrochloric acid; 3 parts of sodium sulfate; 4 parts of triethanolamine; and 6 parts of glycerol.
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