CN108059376B - Preparation method of dental model gypsum - Google Patents
Preparation method of dental model gypsum Download PDFInfo
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- CN108059376B CN108059376B CN201711484360.3A CN201711484360A CN108059376B CN 108059376 B CN108059376 B CN 108059376B CN 201711484360 A CN201711484360 A CN 201711484360A CN 108059376 B CN108059376 B CN 108059376B
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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
- C04B11/00—Calcium sulfate cements
- C04B11/26—Calcium sulfate cements strating from chemical gypsum; starting from phosphogypsum or from waste, e.g. purification products of smoke
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
- A61C13/00—Dental prostheses; Making same
- A61C13/34—Making or working of models, e.g. preliminary castings, trial dentures; Dowel pins [4]
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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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/14—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements
- C04B28/145—Calcium sulfate hemi-hydrate with a specific crystal form
- C04B28/146—Calcium sulfate hemi-hydrate with a specific crystal form alpha-hemihydrate
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00836—Uses not provided for elsewhere in C04B2111/00 for medical or dental applications
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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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dentistry (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
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- Dental Preparations (AREA)
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Abstract
The invention provides a preparation method of dental model gypsum, which comprises the steps of mixing and stirring 100 parts of high-purity high-whiteness alpha-type semi-hydrated gypsum powder obtained by a liquid phase method, 15-20 parts of a reinforcing agent, 10-12 parts of a toughening agent, 8-10 parts of an anti-wear agent, 6-8 parts of a water reducing agent and 3-5 parts of a defoaming agent, and then molding, wherein the reinforcing agent is cyanoacrylate, the toughening agent is polypropylene resin and fiber, the anti-wear agent is a copolymer of butadiene and acrylonitrile, the water reducing agent is a naphthalene high-efficiency water reducing agent and melamine, and the defoaming agent is a D-30X high-efficiency defoaming agent. The preparation method of the dental model gypsum provided by the invention adopts a new formula and dosage, overcomes the defects of small strength and hardness of the original dental gypsum, and simultaneously improves the toughness and wear resistance of the finished gypsum product.
Description
Technical Field
The invention relates to a plaster, in particular to a preparation method of a dental model plaster.
Background
The dental plaster is an indispensable model reproducing material in the process of dentist diagnosis clinical operation and treatment, can enable dentists to diagnose and treat outside the oral cavity of a patient, and is an important medical material. The medical dental gypsum has higher requirements on the performances of the gypsum such as hardness, density, strength and the like, but the performances of the existing dental gypsum are difficult to meet the requirements.
The invention patent of application number 201210000045.X discloses dental gypsum in 'a dental high-strength gypsum', which comprises 100 parts of alpha-hemihydrate gypsum powder; 3-10 parts of a reinforcing agent; 2-7 parts of a water reducing agent; 0-5 parts of cement are uniformly mixed to prepare the cement. The invention adopts the mode of adding the additive into the common alpha-semi-hydrated gypsum to improve the setting performance of the gypsum and improve the density, the strength and the hardness of the gypsum. However, the performance of the gypsum is still insufficient, the strength and hardness of the gypsum finished product are still insufficient, and the toughness, abrasion resistance and the like of the gypsum finished product can not meet the requirements.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of dental model gypsum, which adopts a new formula and dosage, improves the defects of small strength and hardness of the original dental gypsum and improves the toughness and wear resistance of the finished gypsum product.
The invention is realized by the following steps:
the invention provides a preparation method of dental model plaster, which comprises the following steps:
step 2, crystal transformation reaction: and (2) placing the gypsum powder into a slurry mixer, wherein the solid-to-liquid ratio is 1: 8, adding the sulfuric acid and the phosphoric acid into a mixed acid aqueous solution according to the proportion, and uniformly mixing to obtain mixed slurry, wherein the mass of the sulfuric acid is 8-10% of the total mass of the mixed acid aqueous solution in terms of H2SO4, the mass of the phosphoric acid is 18-20% of the total mass of the mixed acid aqueous solution in terms of P2O5, 0.1-5% of a crystal transformation agent is added, the crystal transformation agent comprises a mixture of sodium citrate, potassium glutarate, magnesium succinate and inorganic salts, and then 1-6% of sodium acetate in mass percentage is added as an additive to form a supersaturated solution system, the slurry is kept at 80-120 ℃ for crystal transformation reaction, and the transformation reaction time is 4-16 hours;
step 3, directional crystallization: adding 0.1% of crystal form control agent into the mixed slurry, uniformly stirring, carrying out directional crystallization for 1-4 h to obtain a mixed solution containing alpha-type semi-hydrated gypsum, wherein the crystal form control agent comprises fumaric acid, fatty acid and a surfactant;
and 4, separating by a liquid phase method: carrying out solid-liquid separation on the mixed solution containing the alpha-type semi-hydrated gypsum prepared in the step (3) to obtain a solid phase A and a liquid phase B, and recycling the liquid phase B;
step 5, washing and separating: mixing the solid phase A and the liquid phase B obtained in the step (4) for a circulating crystal transformation reaction, and washing the solid phase A with hot water at the temperature of 80-100 ℃ to obtain a solid phase C and a liquid phase D; and the liquid phase D is used for diluting concentrated sulfuric acid to provide a sulfuric acid solution, and the solid phase C is dried to obtain pure alpha-type semi-hydrated gypsum crystals.
Step 6, drying and grinding: and (3) drying the pure alpha-type semi-hydrated gypsum crystal obtained in the step (5) at 120-170 ℃, drying, and grinding according to application fineness to obtain high-purity high-whiteness alpha-type semi-hydrated gypsum powder.
Step 7, preparing a dental model gypsum raw material: reinforcing agent, toughening agent, antiwear agent, water reducing agent, defoaming agent and the alpha-type semi-hydrated gypsum powder obtained in the step 11, wherein the dental model gypsum comprises the following raw materials in parts by weight: 100 parts of alpha-type semi-hydrated gypsum powder, 15-20 parts of a reinforcing agent, 10-12 parts of a toughening agent, 8-10 parts of an antiwear agent, 6-8 parts of a water reducing agent and 3-5 parts of a defoaming agent, wherein the reinforcing agent is cyanoacrylate, the toughening agent is polypropylene resin and fiber, the antiwear agent is a copolymer of butadiene and acrylonitrile, the water reducing agent is a naphthalene-based high-efficiency water reducing agent and melamine, and the defoaming agent is a D-30X high-efficiency defoaming agent.
Step 8, stirring: adding water with a proper proportion, manually stirring for 30-40 seconds or manually stirring for 10-15 seconds, and then stirring in vacuum for 20-30 seconds;
step 9, molding: pouring the finished product after vacuum stirring into the impression to replicate the model, standing for 10-15 minutes, and removing after curing.
The invention has the following beneficial effects:
the invention provides a preparation method of dental model gypsum, which adopts a new formula and dosage, wherein the dental model gypsum comprises the following raw materials in parts by weight: 100 parts of alpha-type semi-hydrated gypsum powder, 15-20 parts of reinforcing agent, 10-12 parts of toughening agent, 8-10 parts of antiwear agent, 6-8 parts of water reducing agent and 3-5 parts of defoaming agent, so that the defects of small strength and hardness of the original dental gypsum are overcome, and the toughness and the abrasion resistance of the finished gypsum product are improved.
Drawings
Fig. 1 is a process flow chart of a method for preparing dental model plaster according to an embodiment of the present invention.
Detailed Description
Example 1
As shown in fig. 1, an embodiment of the present invention provides a method for preparing a dental model plaster, including the following steps:
step 2, crystal transformation reaction: and (2) placing the gypsum powder into a slurry mixer, wherein the solid-to-liquid ratio is 1: 8, adding the sulfuric acid and the phosphoric acid into a mixed acid aqueous solution according to the proportion, and uniformly mixing to prepare a mixed slurry, wherein the mass of the sulfuric acid is 9.00 percent of the mass of the mixed acid calculated by H2SO4, the mass of the phosphoric acid is 20.00 percent of the mass of the mixed acid calculated by P2O5, the mass of the added water is 34.79 percent of the mass of the mixed acid aqueous solution, adding a crystal transformation agent into the mixed slurry, uniformly stirring, and carrying out crystal transformation reaction at 100 ℃ for 3 hours to obtain a mixed solution containing alpha-type hemihydrate gypsum, wherein the crystal transformation agent is a mixture of sodium sulfate, sodium citrate, potassium glutarate and magnesium succinate, the adding amount of the sodium sulfate is 0.2 percent of the total mass of the mixed acid aqueous solution, the adding amount of the sodium citrate is 0.1 percent of the total mass of the mixed acid aqueous solution, the adding amount of the potassium glutarate is 0.1 percent of the total mass of the mixed acid aqueous solution, and the adding amount of the magnesium succinate is 0.1 percent of the.
Step 3, directional crystallization: adding 0.1% of crystal form control agent into the mixed slurry, uniformly stirring, carrying out directional crystallization for 1-4 h to obtain a mixed solution containing alpha-type semi-hydrated gypsum, wherein the crystal form control agent comprises 40% of fumaric acid, 50% of fatty acid and 10% of sodium dodecyl benzene sulfonate;
and 4, separating by a liquid phase method: carrying out solid-liquid separation on the mixed solution containing the alpha-type semi-hydrated gypsum prepared in the step (3) to obtain a solid phase A and a liquid phase B, and recycling the liquid phase B;
step 5, washing and separating: mixing the solid phase A and the liquid phase B obtained in the step (4) for a circulating crystal transformation reaction, and washing the solid phase A with hot water at the temperature of 80-100 ℃ to obtain a solid phase C and a liquid phase D; and the liquid phase D is used for diluting concentrated sulfuric acid to provide a sulfuric acid solution, and the solid phase C is dried to obtain pure alpha-type semi-hydrated gypsum crystals.
And (3) carrying out related performance measurement on the prepared pure alpha-type semi-hydrated gypsum crystal:
the alpha-type semi-hydrated gypsum product prepared in the embodiment 1 meets the JC/T2038-2010 industry standard, is in a hexagonal short column shape under an optical microscope of 200 times, and has the length-diameter ratio of 1-2, the 2h flexural strength of 20MPa, the dry compressive strength of 120MPa, the initial setting in 7 minutes and the final setting in 15 minutes.
Step 6, drying and grinding: and (3) drying the pure alpha-type semi-hydrated gypsum crystal obtained in the step (5) at 120-170 ℃, drying, and grinding according to application fineness to obtain high-purity high-whiteness alpha-type semi-hydrated gypsum powder.
Step 7, preparing a dental model gypsum raw material: reinforcing agent, toughening agent, antiwear agent, water reducing agent, defoaming agent and the alpha-type semi-hydrated gypsum powder obtained in the step 11, wherein the dental model gypsum comprises the following raw materials in parts by weight: 100 parts of alpha-type semi-hydrated gypsum powder, 20 parts of reinforcing agent, 12 parts of toughening agent, 10 parts of antiwear agent, 8 parts of water reducing agent and 5 parts of defoaming agent, wherein the reinforcing agent is cyanoacrylate, the toughening agent is polypropylene resin and fiber, the antiwear agent is a copolymer of butadiene and acrylonitrile, the water reducing agent is naphthalene-based high-efficiency water reducing agent and melamine, and the defoaming agent is D-30X high-efficiency defoaming agent.
Step 8, stirring: adding water with a proper proportion, manually stirring for 30-40 seconds or manually stirring for 10-15 seconds, and then stirring in vacuum for 20-30 seconds;
step 9, molding: pouring the finished product after vacuum stirring into the impression to replicate the model, standing for 10-15 minutes, and removing after curing.
Example 2
The embodiment of the invention provides a preparation method of dental model plaster, steps 1-6 and steps 8-9 are the same as those in embodiment 1, and different:
step 7, preparing a dental model gypsum raw material: reinforcing agent, toughening agent, antiwear agent, water reducing agent, defoaming agent and the alpha-type semi-hydrated gypsum powder obtained in the step 11, wherein the dental model gypsum comprises the following raw materials in parts by weight: 100 parts of alpha-type semi-hydrated gypsum powder, 15 parts of reinforcing agent, 10 parts of toughening agent, 8 parts of antiwear agent, 6 parts of water reducing agent and 3 parts of defoaming agent, wherein the reinforcing agent is cyanoacrylate, the toughening agent is polypropylene resin and fiber, the antiwear agent is a copolymer of butadiene and acrylonitrile, the water reducing agent is naphthalene-based high-efficiency water reducing agent and melamine, and the defoaming agent is D-30X high-efficiency defoaming agent.
Example 3
The embodiment of the invention provides a preparation method of dental model plaster, steps 1-6 and steps 8-9 are the same as those in embodiment 1, and different:
step 7, preparing a dental model gypsum raw material: reinforcing agent, toughening agent, antiwear agent, water reducing agent, defoaming agent and the alpha-type semi-hydrated gypsum powder obtained in the step 11, wherein the dental model gypsum comprises the following raw materials in parts by weight: 100 parts of alpha-type semi-hydrated gypsum powder, 18 parts of reinforcing agent, 11 parts of toughening agent, 9 parts of antiwear agent, 7 parts of water reducing agent and 4 parts of defoaming agent, wherein the reinforcing agent is cyanoacrylate, the toughening agent is polypropylene resin and fiber, the antiwear agent is a copolymer of butadiene and acrylonitrile, the water reducing agent is naphthalene-based high-efficiency water reducing agent and melamine, and the defoaming agent is D-30X high-efficiency defoaming agent.
The finished dental model plasters of example 1, example 2 and example 3 were tested and the existing dental plasters were used as comparative examples and the properties are shown in the following table:
| item | Compressive strength | Flexural strength | Relative abrasion resistance | Expansion ratio | Curing time |
| Example 1 | 62MPa | 20MPa | 1.064 | 0.1％ | 10-15min |
| Example 2 | 70MPa | 22MPa | 1.014 | 0.1％ | 10-15min |
| Example 3 | 65MPa | 20MPa | 1.004 | 0.1％ | 10-15min |
| Comparative example | 20MPa | 10MPa | 0.464 | 0.2％ | 15-20min |
It can be seen that, the indexes of compressive strength, flexural strength, abrasion resistance, expansion rate and the like in the three embodiments are greatly improved compared with the prior art, the required water is correspondingly reduced, particularly, the expansion rate is greatly reduced compared with the prior art, the expansion of gypsum in the manufacturing process is greatly reduced, the detachment of a gypsum mold is convenient, and the possibility of gypsum breakage is reduced due to the higher flexural strength and compressive strength.
Those not described in detail in this specification are within the skill of the art.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (2)
1. A preparation method of dental model plaster is characterized by comprising the following steps:
step 1, purification treatment: preparing phosphogypsum into slurry with solid content of 5-60%, filtering out large impurities and suspended matters by using a screen, adding dilute sulfuric acid (1-12M) for neutralization reaction, removing a small amount of insoluble oxides, calcium carbonate, magnesium carbonate and other impurities to convert the impurities into soluble salt, filtering out organic carbon, adding quicklime for neutralization treatment, crushing and grinding into gypsum powder with fineness and particle distribution D50 between 20-50 um;
step 2, crystal transformation reaction: and (2) placing the gypsum powder into a slurry mixer, wherein the solid-to-liquid ratio is 1: 8, adding the sulfuric acid and the phosphoric acid into a mixed acid aqueous solution according to the proportion, and uniformly mixing to obtain mixed slurry, wherein the mass of the sulfuric acid is 8-10% of the total mass of the mixed acid aqueous solution in terms of H2SO4, the mass of the phosphoric acid is 18-20% of the total mass of the mixed acid aqueous solution in terms of P2O5, 0.1-5% of a crystal transformation agent is added, the crystal transformation agent comprises a mixture of sodium citrate, potassium glutarate, magnesium succinate and inorganic salts, and then 1-6% of sodium acetate in mass percentage is added as an additive to form a supersaturated solution system, the slurry is kept at 80-120 ℃ for crystal transformation reaction, and the transformation reaction time is 4-16 hours;
step 3, directional crystallization: adding 0.1% of crystal form control agent into the mixed slurry, uniformly stirring, carrying out directional crystallization for 1-4 h to obtain a mixed solution containing alpha-type semi-hydrated gypsum, wherein the crystal form control agent comprises fumaric acid, fatty acid and a surfactant;
and 4, separating by a liquid phase method: carrying out solid-liquid separation on the mixed solution containing the alpha-type semi-hydrated gypsum prepared in the step (3) to obtain a solid phase A and a liquid phase B, and recycling the liquid phase B;
step 5, washing and separating: mixing the solid phase A and the liquid phase B obtained in the step (4) for a circulating crystal transformation reaction, and washing the solid phase A with hot water at the temperature of 80-100 ℃ to obtain a solid phase C and a liquid phase D; the liquid phase D is used for diluting concentrated sulfuric acid to provide sulfuric acid solution, and the solid phase C is dried to obtain pure alpha-type semi-hydrated gypsum crystals;
step 6, drying and grinding: drying the pure alpha-type semi-hydrated gypsum crystal obtained in the step (5) at 120-170 ℃, drying and grinding according to application fineness to obtain high-purity high-whiteness alpha-type semi-hydrated gypsum powder;
step 7, preparing a dental model gypsum raw material: reinforcing agent, toughening agent, antiwear agent, water reducing agent, defoaming agent and the alpha-type semi-hydrated gypsum powder obtained in the step 6, wherein the dental model gypsum comprises the following raw materials in parts by weight: 100 parts of alpha-type semi-hydrated gypsum powder, 15-20 parts of a reinforcing agent, 10-12 parts of a toughening agent, 8-10 parts of an antiwear agent, 6-8 parts of a water reducing agent and 3-5 parts of a defoaming agent, wherein the reinforcing agent is cyanoacrylate, the toughening agent is polypropylene resin and fiber, the antiwear agent is a copolymer of butadiene and acrylonitrile, the water reducing agent is a naphthalene-based high-efficiency water reducing agent and melamine, and the defoaming agent is a D-30X high-efficiency defoaming agent;
step 8, stirring: adding water with a proper proportion, manually stirring for 30-40 seconds or manually stirring for 10-15 seconds, and then stirring in vacuum for 20-30 seconds;
step 9, molding: pouring the finished product after vacuum stirring into a die to reproduce the model, standing for 10-15 minutes, and removing after curing;
the inorganic salt in the step 2 is sodium sulfate, the addition amount of the sodium sulfate accounts for 0.2 percent of the total mass of the mixed acid aqueous solution, the addition amount of the sodium citrate accounts for 0.1 percent of the total mass of the mixed acid aqueous solution, the addition amount of the potassium glutarate accounts for 0.1 percent of the total mass of the mixed acid aqueous solution, and the addition amount of the magnesium succinate accounts for 0.1 percent of the total mass of the mixed acid aqueous solution;
the surfactant in the step 3 is sodium dodecyl benzene sulfonate, and the crystal form control agent comprises 40% of fumaric acid, 50% of fatty acid and 10% of sodium dodecyl benzene sulfonate.
2. The method of claim 1, wherein the fibers of step 7 are one or more of glass fibers, polyester fibers, or asbestos fibers.
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| CN113666704A (en) * | 2021-08-23 | 2021-11-19 | 深圳市青青源科技有限公司 | Method for improving powder falling of dental gypsum |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101734871A (en) * | 2008-11-18 | 2010-06-16 | 北京建筑材料科学研究总院有限公司 | Method for preparing alpha semi-hydrated gypsum by utilizing desulfurized gypsum |
| CN105174760A (en) * | 2015-09-18 | 2015-12-23 | 金正大生态工程集团股份有限公司 | Method for preparing alpha semi-hydrated gypsum from dihydrate gypsum |
| CN105198343A (en) * | 2015-08-29 | 2015-12-30 | 湖北凯浩鹿宝石膏科技有限公司 | Ultrahigh hardness gypsum for dental department and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101734871A (en) * | 2008-11-18 | 2010-06-16 | 北京建筑材料科学研究总院有限公司 | Method for preparing alpha semi-hydrated gypsum by utilizing desulfurized gypsum |
| CN105198343A (en) * | 2015-08-29 | 2015-12-30 | 湖北凯浩鹿宝石膏科技有限公司 | Ultrahigh hardness gypsum for dental department and preparation method thereof |
| CN105174760A (en) * | 2015-09-18 | 2015-12-23 | 金正大生态工程集团股份有限公司 | Method for preparing alpha semi-hydrated gypsum from dihydrate gypsum |
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