CN102776569A - Method for preparing calcium sulfate crystal whiskers by using natural gypsum - Google Patents

Method for preparing calcium sulfate crystal whiskers by using natural gypsum Download PDF

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CN102776569A
CN102776569A CN2012102373746A CN201210237374A CN102776569A CN 102776569 A CN102776569 A CN 102776569A CN 2012102373746 A CN2012102373746 A CN 2012102373746A CN 201210237374 A CN201210237374 A CN 201210237374A CN 102776569 A CN102776569 A CN 102776569A
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calcium sulfate
plaster
paris
reaction
crystal whiskers
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杨荣华
杨明晖
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Taishan Medical University
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Taishan Medical University
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Abstract

The invention belongs to the technical field of chemical production and provides a method for preparing calcium sulfate crystal whiskers by using natural gypsum. The method comprises the steps of: firstly treating and purifying the natural gypsum by adopting a chemical method, enabling the natural gypsum to have double decomposition reaction with ammonium hydrogen carbonate and ammonia water to obtain ammonium sulfate and calcium carbonate, conducting solid-liquid separation to obtain ammonium sulfate solution and crude calcium carbonate, using hydrochloric acid to treat the byproduct crude calcium carbonate to obtain calcium chloride solution, removing impurities, and enabling the calcium chloride to react with the ammonium sulfate to obtain pure calcium sulfate; and then preparing the calcium sulfate crystal whiskers through a hydrothermal method by using the purified calcium sulfate. The method for preparing the calcium sulfate crystal whiskers by using the natural gypsum has the advantages that since the rich natural gypsum and low-cost chemical raw materials are used for producing high-added-value chemical products calcium sulfate crystal whiskers and byproducts ammonium chloride and carbon dioxide, the raw materials are fully utilized, the production cost is effectively reduced, the production process is clean and environmental-friendly, and the promotion and application values are very great.

Description

A kind of method of utilizing the plaster of paris to prepare calcium sulfate crystal whiskers
Technical field
The invention belongs to chemical production technical field, relate in particular to a kind of method of utilizing the plaster of paris to prepare calcium sulfate crystal whiskers.
Background technology
The plaster of paris is one of advantage mineral products of China; Explored reserves have 1,000 hundred million tons, rank first in the world about about 2,000 ten thousand tons of the plaster of paris that exploitation is at present come out; Wherein 80% is used for Cement industry and makes cement setting retarder, is used for agricultural, medical, chemical industry etc. and only accounts for about 15%.The chemical utilization of China's plaster of paris and deep process technology are compared with advanced country in the world has bigger gap.Therefore, make full use of the resources advantage of China, the deep process technology of development gypsum product, the Chemicals of production high-performance and high added value are problems being badly in need of solution at present.
Whisker be meant have the fixed shape of cross section, complete profile, perfect internal structure, length-to-diameter ratio be up to 5~1000 fibrous single crystal; Its intensity can be the very excellent advanced composite material strengthening and toughening agent of one type of mechanical property near the theoretical value of perfect crystal material.The diameter dimension of whisker is between micron and hundred nano-scale, because the atomic arrangement structure of its high-sequential, makes its intensity and modulus approach the theoretical strength of valence link between the atom of material, and this makes the physics of whisker, chemical property excellent especially.
Calcium sulfate crystal whiskers (CSW) be crystal whisker of gypsum again, is CaSO 4Fibrous single crystal, the same branch with gypsum with anhydrous, Ban Shui and two water.Moisture whisker can only be lower than 176.7 ℃ of uses down, and the use temperature of anhydrous whisker is up to 1000 ℃, thereby CSW anhydrous and half water has than hard intensity and higher use value.The dimensional stabilizing of calcium sulfate crystal whiskers, average aspect ratio are 80, and that calcium sulfate crystal whiskers has is high temperature resistant, resist chemical, good toughness, intensity are high, be prone to carry out advantages such as the avidity of polymkeric substance such as surface treatment and rubber plastic is strong.Compare with other whiskers, except that having good enhancing and modification function, also have the low and minimum characteristics of toxicity of production cost, it is routine to have very strong market competition.Calcium sulfate crystal whiskers is because its particular structural characteristic makes it at aspects such as various matrix materials, water technology, road modified asphalt, fire-retardant fireproof material, papermaking, coating, paint application promise in clinical practice arranged all.Calcium sulfate crystal whiskers can be used as the weighting agent of medium tenacity, and the reinforcing effect of the reinforcing effect of small diameter fiber and other high-performance fiber strongtheners is approaching; With its enhanced plastics, tensile strength, flexural strength, crooked elastic rate and heat-drawn wire are improved; It can replace asbestos to make friction materials, material of construction, and insulation, cold insulation material etc. can also partly replace spun glass.
Open about the existing multinomial patent of Preparation methods of gypsum whiskers.Chinese patent publication number CN1955345A discloses on May 2nd, 2007 " Preparation methods of gypsum whiskers method ", and this method adopts the synthetic crystallization directors of technology such as hydrothermal synthesis method; The pre-treatment of technical grade quicklime elder generation, put into reactor drum 40~60 ℃ of digestion; Obtain lime slurry, the gained lime slurry is warming up to 40~110 ℃ in reactor drum, add equimolar sulphuric acid soln; Stir 30~60min; In the process of reaction, add crystallization director, it is fully reacted, obtain required calcium sulfate crystal whiskers product through filtration, washing, surface treatment and drying.This invention is a raw material with quicklime and sulfuric acid, and complex technical process and cost are higher.Chinese patent publication number CN1598083A; Disclose on March 23rd, 2005 " Preparation methods of gypsum whiskers method "; This method is a raw material with plaster stone and water, through raw material preparation, building-up reactions, dehydrate and an operation such as refining and edulcoration, it is characterized in that the effective content of selected raw material plaster stone reaches more than 95%, whiteness is more than 90%; With the mixed plaster stone slip that gets of tap water; After fully emulsified, add and to make it that chemical reaction takes place in the reactor drum, and then enter into later operation and make the calcium sulfate crystal whiskers product.It is raw material that this patent adopts the higher plaster stone of purity, is not suitable for adopting containing the more plaster of paris raw material of impurity.Chinese patent publication number CN10132397A; Disclose on December 17th, 2008 " a kind of method for preparing calcium sulfate crystal whiskers from scud "; This method is raw material with scud, prepares calcium sulfate crystal whiskers through steps such as ore acidifying, the synthetic crystal seed of microwave, the synthetic whiskers of hydro-thermal.
Chinese patent publication number CN101792932A; Disclose on August 4th, 2010 " a kind of method for preparing ultra-fine calcium sulfate crystal whisker by phosphogypsum "; This method is 0.1~100 μ m with phosphogypsum ultrafining treatment to particle diameter; Through hydrothermal synthesis reaction, filtration, dry preparation calcium sulfate crystal whiskers, and add the crystal formation growth substance to improve its performance.Chinese patent publication number CN101311355A; Disclose on November 26th, 2008 " a kind of method of preparing calcium sulphate whiskers from ardealite "; This method uses the solid slag phosphogypsum to be raw material; Preparing diameter of whiskers through synthetic reaction, filtration, heating for dissolving, heat filtering and crystallisation by cooling is 1~4 μ m, length 50~200 μ m, the calcium sulfate crystal whiskers product of diameter and length controlled.This method raw material phosphogypsum is without any processing, and the product calcium sulfate crystal whiskers does not pass through any modification yet, and the calcium sulfate crystal whiskers length-to-diameter ratio of preparing is little.
Summary of the invention
The invention provides a kind of method of utilizing the plaster of paris to prepare calcium sulfate crystal whiskers; Be intended to solve the method for preparing calcium sulfate crystal whiskers that prior art provides; To having relatively high expectations of raw material, raw material can not be fully used, the inferior quality of the calcium sulfate crystal whiskers of preparing; Production cost is higher, the problem that environmental pollution is comparatively serious.
The object of the present invention is to provide a kind of method of utilizing the plaster of paris to prepare calcium sulfate crystal whiskers, this method may further comprise the steps:
Adopt chemical process that the plaster of paris is purified and purification processes;
Calcium sulfate to the plaster of paris purifies and purification processes obtains adopts the Hydrothermal Preparation calcium sulfate crystal whiskers.
Further, adopt chemical process that the plaster of paris is purified and the implementation method of purification processes is:
The plaster of paris and bicarbonate of ammonia, ammoniacal liquor are carried out replacement(metathesis)reaction obtain ammonium sulfate and lime carbonate, after solid-liquid separation, obtain ammoniumsulphate soln and bullion lime carbonate;
Obtain calcium chloride solution and remove impurity with salt s.t. bullion lime carbonate, calcium chloride and ammonium sulfate reaction are obtained pure calcium sulfate and sub product ammonium chloride.
Further, the processing condition that the plaster of paris and bicarbonate of ammonia, ammoniacal liquor carry out replacement(metathesis)reaction are: 45~60 ℃ of temperature of reaction, reaction times 1~2h, ratio of components: CaSO 42H 2O: NH 4HCO 3: NH 3H 2O: H 2The mol ratio of O=1: 1.1: 1.2: 15; Bullion lime carbonate uses the processing condition of salt s.t. to be: 20~30 ℃ of temperature of reaction, and reaction times 20~30min, concentration of hydrochloric acid 2.5mol/L, the batching mol ratio is HCl: CaCO 3=2.5: 1.
Further, the plaster of paris is purified and calcium sulfate that purification processes obtains adopts the processing condition of Hydrothermal Preparation calcium sulfate crystal whiskers to be: the initial pH of 120~140 ℃ of temperature of reaction, slip 8.0~10.0, pulp quality mark 3%~5%, reaction times 1.0~2.0h.
Further, it is that 1.32 μ m, length-to-diameter ratio are 76~90 that the calcium sulfate that the plaster of paris purifies and purification processes obtains adopts the mean diameter of Hydrothermal Preparation calcium sulfate crystal whiskers.
The method of utilizing the plaster of paris to prepare calcium sulfate crystal whiskers provided by the invention; At first adopt chemical process that the plaster of paris is carried out purifying treatment and purification; The plaster of paris and bicarbonate of ammonia, ammoniacal liquor are carried out replacement(metathesis)reaction obtain ammonium sulfate and lime carbonate; After solid-liquid separation, obtain ammoniumsulphate soln and bullion lime carbonate, obtain calcium chloride solution and remove impurity, calcium chloride and ammonium sulfate reaction are obtained pure calcium sulfate with the bullion lime carbonate of salt s.t. by-product; The calcium sulfate that then purification is obtained adopts the Hydrothermal Preparation calcium sulfate crystal whiskers; Chemicals calcium sulfate crystal whiskers that plaster of paris resource that this method utilization for preparing calcium sulfate crystal whiskers is enriched and cheap industrial chemicals obtain high added value and sub product ammonium chloride, carbonic acid gas; Raw material is fully used; Reduce production costs; The production process clean environment firendly has stronger popularization and using value.
Description of drawings
Fig. 1 is that the plaster of paris that utilizes that the embodiment of the invention provides prepares the realization flow figure of the method for calcium sulfate crystal whiskers.
Embodiment
In order to make the object of the invention, technical scheme and advantage clearer,, the present invention is further specified below in conjunction with accompanying drawing and embodiment.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in the qualification invention.
The plaster of paris that utilizes that Fig. 1 shows the embodiment of the invention to be provided prepares the realization flow of the method for calcium sulfate crystal whiskers.This method may further comprise the steps:
In step S101, adopt chemical process that the plaster of paris is purified and purification processes;
In step S102, the calcium sulfate that the plaster of paris purifies and purification processes obtains is adopted the Hydrothermal Preparation calcium sulfate crystal whiskers.
In embodiments of the present invention, at first be raw material with the plaster of paris, adopt chemical process that the plaster of paris is carried out purifying treatment and purification, adopt the Hydrothermal Preparation calcium sulfate crystal whiskers then;
The plaster of paris and bicarbonate of ammonia, ammoniacal liquor are carried out replacement(metathesis)reaction obtain ammonium sulfate and lime carbonate; After solid-liquid separation, obtain ammoniumsulphate soln and bullion lime carbonate; Lime carbonate bullion with salt s.t. by-product obtains calcium chloride solution and removes impurity; Calcium chloride and ammonium sulfate reaction are obtained pure calcium sulfate, and side product sodium chloride, adopt hydrothermal method to synthesize calcium sulfate crystal whiskers then.
The suitable processing condition of plaster of paris purifying treatment are: 45~60 ℃ of temperature of reaction, reaction times 1~2h, ratio of components: CaSO 42H 2O: NH 4HCO 3: NH 3H 2O: H 2The mol ratio of O=1: 1.1: 1.2: 15, to react with this understanding, reaction obtains ammonium sulfate liquor and lime carbonate bullion with material filtering after finishing; By product bullion lime carbonate is handled with industrial by-product hydrochloric acid, and this reaction appropriate processing condition is: 20~30 ℃ of temperature of reaction, reaction times 20~30min, concentration of hydrochloric acid 2.5mol/L, batching mol ratio are 2.5: 1, reclaim the CO that reaction process produces 2, reaction finishes after insoluble impurities is removed in filtration, obtains ammonium chloride mother liquor; Above-mentioned gained ammonium sulfate and calcium chloride obtain calcium sulfate and ammonium chloride according to the reaction of 1: 1 ratio of mol ratio under normal temperature condition, obtain the higher calcium sulfate of purity through solid-liquid separation, and ammonium chloride obtains ammonia chloride crystal through evaporation, drying; With gained calcium sulfate is raw material; Adopt the Hydrothermal Preparation calcium sulfate crystal whiskers; Temperature of reaction is that 120~140 ℃, the initial pH of slip are 8.0~10.0, the pulp quality mark is 3%~5%, the reaction times is 1.0~2.0h, and obtaining mean diameter is that 1.2 μ m, length-to-diameter ratio are 76~90 calcium sulfate crystal whiskers product.
Instance 1: the 86g plaster of paris is removed partial impurities through rinsing earlier; Be added in the reactor drum then; Add 130ml circulate soln or water, start stirring and be heated to 45 ℃, add 40g bicarbonate of ammonia and 35ml ammoniacal liquor in batches; Stirring reaction 60min final vacuum suction filtration obtains ammoniumsulphate soln and lime carbonate bullion.Get 64g lime carbonate bullion, add the hydrochloric acid soln of 300ml 2.5mol/L,, reclaim the CO that reaction generates at 20~30 ℃ of following stirring reaction 20~30min 2Gas, reaction finish after-filtration and remove impurity, obtain calcium chloride solution; Gained ammonium sulfate and calcium chloride solution according to its concentration, according to hybrid reaction under 1: 1 the mol ratio normal temperature, are obtained calcium sulfate precipitation and ammonium chloride solution through filtering to separate; Get the calcium sulfate after the 5g purifying treatment, add 95g water, after stirring; Regulating PH is 9~10, is placed in the hydrothermal reactor, reacts 1.5h down at 130 ℃; Filtered while hot; Obtain calcium sulfate crystal whiskers 200 ℃ of dryings, using the diameter of scanning electron microscopic observation whisker is 1.2 μ m, and length-to-diameter ratio is 76~85.
Instance 2: the 1000g plaster of paris is removed partial impurities through rinsing earlier, be added to then in the reaction kettle, add 2000ml circulate soln or water; Start stirring and be heated to 55 ℃; Add 610g bicarbonate of ammonia and 550ml ammoniacal liquor, stirring reaction 1h is warmed up to 60 ℃ and continues stirring reaction 1h in batches; Reaction finishes the final vacuum suction filtration, obtains ammoniumsulphate soln and lime carbonate bullion.Get 110g lime carbonate bullion, add the hydrochloric acid soln of 540ml 2.5mol/L,, reclaim the CO that reaction generates at 20~30 ℃ of following stirring reaction 20~30min 2Gas, reaction finish after-filtration and remove impurity, obtain calcium chloride solution.Gained ammonium sulfate and calcium chloride solution according to its concentration, according to hybrid reaction under 1: 1 the mol ratio normal temperature, are obtained calcium sulfate precipitation and ammonium chloride solution through filtering to separate.Get the calcium sulfate after the 300g purifying treatment, add 6000ml water, after stirring; Regulating PH is 9~10, is placed in the 10L reaction kettle, reacts 2.0h down at 130 ℃; Filtered while hot; Obtain calcium sulfate crystal whiskers 200 ℃ of dryings, using the diameter of scanning electron microscopic observation whisker is 1.2 μ m, and length-to-diameter ratio is 85~90.
The above is merely preferred embodiment of the present invention, not in order to restriction the present invention, all any modifications of within spirit of the present invention and principle, being done, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.

Claims (5)

1. a method of utilizing the plaster of paris to prepare calcium sulfate crystal whiskers is characterized in that, this method may further comprise the steps:
Adopt chemical process that the plaster of paris is purified and purification processes;
Calcium sulfate to the plaster of paris purifies and purification processes obtains adopts the Hydrothermal Preparation calcium sulfate crystal whiskers.
2. the method for claim 1 is characterized in that, the plaster of paris is purified the employing chemical process and the implementation method of purification processes is:
The plaster of paris and bicarbonate of ammonia, ammoniacal liquor are carried out replacement(metathesis)reaction obtain ammonium sulfate and lime carbonate, after solid-liquid separation, obtain ammoniumsulphate soln and bullion lime carbonate;
Obtain calcium chloride solution and remove impurity with salt s.t. bullion lime carbonate, calcium chloride and ammonium sulfate reaction are obtained pure calcium sulfate and sub product ammonium chloride.
3. the method for claim 1 is characterized in that, the processing condition that the plaster of paris and bicarbonate of ammonia, ammoniacal liquor carry out replacement(metathesis)reaction are: 45~60 ℃ of temperature of reaction, reaction times 1~2h, ratio of components: CaSO 42H 2O: NH 4HCO 3: NH 3H 2O: H 2The mol ratio of O=1: 1.1: 1.2: 15; Bullion lime carbonate uses the processing condition of salt s.t. to be: 20~30 ℃ of temperature of reaction, and reaction times 20~30min, concentration of hydrochloric acid 2.5mol/L, the batching mol ratio is HCl: CaCO 3=2.5: 1.
4. the method for claim 1; It is characterized in that, adopt the processing condition of Hydrothermal Preparation calcium sulfate crystal whiskers to be: the initial pH of 120~140 ℃ of temperature of reaction, slip 8.0~10.0, pulp quality mark 3%~5%, reaction times 1.0~2.0h the calcium sulfate that the plaster of paris purifies and purification processes obtains.
5. method as claimed in claim 4 is characterized in that, it is that 1.32 μ m, length-to-diameter ratio are 76~90 that the calcium sulfate that the plaster of paris purifies and purification processes obtains adopts the mean diameter of Hydrothermal Preparation calcium sulfate crystal whiskers.
CN2012102373746A 2012-07-09 2012-07-09 Method for preparing calcium sulfate crystal whiskers by using natural gypsum Pending CN102776569A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103288118A (en) * 2013-05-24 2013-09-11 东莞上海大学纳米技术研究院 Method for dissociating industrial by-product gypsum and crystallizing to grow calcium sulphate crystal whiskers
CN105040105A (en) * 2015-06-06 2015-11-11 青岛科技大学 Method for preparing calcium sulfate whiskers with oyster shells
CN105220233A (en) * 2015-10-22 2016-01-06 昆明理工大学 A kind of take phosphogypsum as the method that high-purity sulphuric acid calcium pyroborate prepared by raw material
TWI680211B (en) * 2018-10-09 2019-12-21 雷賽克實業股份有限公司 Method of preparing calcium sulfate whiskers
CN110697731A (en) * 2019-11-05 2020-01-17 浙江浙能技术研究院有限公司 Method for preparing ammonium sulfate and calcium carbonate from desulfurized gypsum
CN110965124A (en) * 2019-12-20 2020-04-07 南京工业大学 Method for preparing high-quality calcium sulfate whiskers and calcium oxide by using industrial byproduct gypsum
CN112441607A (en) * 2019-08-28 2021-03-05 西南科技大学 Method for recycling desulfurized gypsum
CN112877780A (en) * 2021-01-14 2021-06-01 江西理工大学 Method for preparing calcium sulfate hemihydrate crystal whisker by ammonia distillation waste liquid hydrothermal method

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103288118A (en) * 2013-05-24 2013-09-11 东莞上海大学纳米技术研究院 Method for dissociating industrial by-product gypsum and crystallizing to grow calcium sulphate crystal whiskers
CN105040105A (en) * 2015-06-06 2015-11-11 青岛科技大学 Method for preparing calcium sulfate whiskers with oyster shells
CN105040105B (en) * 2015-06-06 2019-03-22 青岛科技大学 A method of calcium sulfate crystal whiskers are prepared by oyster shell
CN105220233A (en) * 2015-10-22 2016-01-06 昆明理工大学 A kind of take phosphogypsum as the method that high-purity sulphuric acid calcium pyroborate prepared by raw material
TWI680211B (en) * 2018-10-09 2019-12-21 雷賽克實業股份有限公司 Method of preparing calcium sulfate whiskers
CN112441607A (en) * 2019-08-28 2021-03-05 西南科技大学 Method for recycling desulfurized gypsum
CN110697731A (en) * 2019-11-05 2020-01-17 浙江浙能技术研究院有限公司 Method for preparing ammonium sulfate and calcium carbonate from desulfurized gypsum
CN110965124A (en) * 2019-12-20 2020-04-07 南京工业大学 Method for preparing high-quality calcium sulfate whiskers and calcium oxide by using industrial byproduct gypsum
CN112877780A (en) * 2021-01-14 2021-06-01 江西理工大学 Method for preparing calcium sulfate hemihydrate crystal whisker by ammonia distillation waste liquid hydrothermal method

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Application publication date: 20121114