WO2019165578A1 - Modificateur cristallin et son utilisation pour la préparation de gypse de résistance élevée de type alpha - Google Patents

Modificateur cristallin et son utilisation pour la préparation de gypse de résistance élevée de type alpha Download PDF

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Publication number
WO2019165578A1
WO2019165578A1 PCT/CN2018/077418 CN2018077418W WO2019165578A1 WO 2019165578 A1 WO2019165578 A1 WO 2019165578A1 CN 2018077418 W CN2018077418 W CN 2018077418W WO 2019165578 A1 WO2019165578 A1 WO 2019165578A1
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WIPO (PCT)
Prior art keywords
gypsum
type high
strength
crystallizing agent
strength gypsum
Prior art date
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PCT/CN2018/077418
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English (en)
Chinese (zh)
Inventor
唐永波
唐绍林
万建东
Original Assignee
江苏一夫科技股份有限公司
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Priority to CN201880003981.1A priority Critical patent/CN110023244B/zh
Priority to PCT/CN2018/077418 priority patent/WO2019165578A1/fr
Publication of WO2019165578A1 publication Critical patent/WO2019165578A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/46—Sulfates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/46—Sulfates
    • C01F11/466—Conversion of one form of calcium sulfate to another
    • 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
    • C04B11/02—Methods and apparatus for dehydrating gypsum
    • C04B11/028—Devices therefor characterised by the type of calcining devices used therefor or by the type of hemihydrate obtained
    • C04B11/032—Devices therefor characterised by the type of calcining devices used therefor or by the type of hemihydrate obtained for the wet process, e.g. dehydrating in solution or under saturated vapour conditions, i.e. to obtain alpha-hemihydrate
    • 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
    • C04B24/04—Carboxylic acids; Salts, anhydrides or esters thereof
    • 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

Definitions

  • the invention belongs to the field of deep processing of gypsum, and particularly relates to a crystal conversion agent and the use thereof for preparing ⁇ -type high-strength gypsum.
  • the ⁇ -type high-strength gypsum has excellent mechanical properties and environmental friendliness, and thus has been widely used in self-leveling gypsum mortar, glass fiber reinforced gypsum (GRG products), 3D printing, arts and crafts, and the like.
  • Alpha high-strength gypsum is also a high-quality 3D printing material after proper modification. With 3D printing technology, the preparation of some complex plaster models will be easier. For example, using ⁇ -type high-strength plaster as the printing material to print the bones that are missing due to accidents or diseases, this will revolutionize the medical treatment of orthopedic diseases. Progress in sex.
  • the [001] direction of ⁇ -type high-strength gypsum crystal ( ⁇ -CaSO 4 ⁇ 0.5H 2 O) is composed of Ca 2+ and SO 4 2- ions alternately, which has a honeycomb structure and high surface energy, and ⁇ -type hemihydrate gypsum crystals
  • the Ca 2+ and SO 4 2- ions are “assembled” faster in the [001] direction than in the other directions of the crystal. Therefore, under normal circumstances, dihydrate gypsum grows needle-like crystal-gypsum whiskers under a high-temperature, high-pressure hydrothermal environment.
  • the method is to add a water-soluble organic matter in an aqueous solution, which is a so-called crystallizer, so that the organic matter in the water is adsorbed on the crystal faces of ⁇ -CaSO 4 ⁇ 0.5H 2 O high energy surface-(001) and (114).
  • crystallizer a water-soluble organic matter in an aqueous solution
  • the growth rate of the ⁇ -CaSO 4 ⁇ 0.5H 2 O crystal along the normal direction of the (001) crystal plane is lowered, thereby making it possible to prepare a short columnar ⁇ -CaSO 4 ⁇ 0.5H 2 O crystal.
  • High-performance ⁇ -type high-strength gypsum is generally produced by hydrothermal or semi-dry processes. Whether hydrothermal or semi-dry, a critical additive, a crystallizer, is required in the production process. Therefore, the crystallizer (also known as the crystallizer) has become one of the most critical technologies for the production of high-performance ⁇ -type high-strength gypsum.
  • CN104692442A uses phosphogypsum as raw material to produce ⁇ -type high-strength gypsum by hydrothermal process.
  • the crystal conversion agent used is succinic acid and sodium succinate. And one or more of potassium tartrate);
  • CN104628274A uses sodium citrate and aluminum sulfate as a crystallizing agent to prepare ⁇ high-strength gypsum by autoclaving;
  • CN102992375A is also compounded with sodium citrate and wine gypsum acid and aluminum sulfate.
  • the crystallizer produces ⁇ -type high-strength gypsum
  • CN102615694A uses maleic anhydride and citrate as a crystallizing agent to produce ⁇ -type high-strength gypsum by hydrothermal process
  • CN104556761A uses maleic acid and ethylenediaminetetraacetic acid as crystal
  • the high-strength gypsum with an aspect ratio of about 1:1 was successfully prepared.
  • CN103951297A successfully prepared ⁇ -type ultra-high-strength gypsum gypsum with a dry strength of more than 70 MPa using malic acid as a crystallizing agent.
  • Citric acid and its sodium salt are a common crystal conversion agent for the production of ⁇ -type high-strength gypsum. It has strong crystal-transforming ability and can easily convert dihydrate gypsum into short column-shaped ⁇ -type high strength in hydrothermal or autoclaved environment. Gypsum crystal, but the ⁇ -type high-strength gypsum crystal prepared by using citric acid and its sodium salt as a crystallizing agent affects the morphology of the dihydrate gypsum formed by hydration to some extent due to the presence of citrate during hydration. The dihydrate gypsum crystal formed after the formation tends to become a short and thick flaky dihydrate gypsum crystal.
  • High-strength gypsum strength is also relatively high, but when using succinic acid, malic acid and other substances for high-grade natural gypsum (calcium sulfate content above 85wt%) is not ideal; ethylenediaminetetraacetic acid is very good in crystal transformation Strong, but use it for the most recent When the crystallizer of high-whiteness and high-grade sodium sulphide gypsum newly produced due to technological progress in the phosphate fertilizer industry is still unsatisfactory, in the hydrothermal environment, under the action of ethylenediaminetetraacetic acid, Sulfur gypsum still has no long and short columnar ⁇ -type high-strength gypsum crystals.
  • An object of the present invention is to provide a crystallizing agent which is any one of a compound having a structure of the formula (I), a salt of a compound having a structure of the formula (I), and a compound having a structure of the formula (II).
  • a crystallizing agent which is any one of a compound having a structure of the formula (I), a salt of a compound having a structure of the formula (I), and a compound having a structure of the formula (II).
  • R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 and R 8 are each independently selected from an organic group
  • R' is a methyl group; n is 0 or 1.
  • the crystallizer provided by the invention has two carboxylic acid groups like pliers in water, which can generate strong adsorption on the (114) surface of the ⁇ -CaSO 4 ⁇ 0.5H 2 O crystal (the adsorption energy can reach -1084 kJ/mol); and the gypsum crystal prepared by the crystallizer provided by the present invention has an aspect ratio of about 1:1, and can produce high-strength ⁇ -type high-strength gypsum.
  • the compound having the structure of the formula (I) and the compound having the structure of the formula (II) provided by the present invention are all known compounds, but are mostly used as plasticizers, and are not used as gypsum crystalliners.
  • the salt ion of the salt of the compound having the structure of the formula (I) of the present invention illustratively includes any one or a combination of at least two of sodium ion, potassium ion and ammonium ion.
  • the solubility of the salt of the compound having the structure of the formula (I) and the salt of the compound having the structure of the formula (II) is 0.005 g/L or more (for example, 0.005 g/L, 0.008 g/L, 0.010 g/L). , 0.015g / L, 0.030g / L, 0.040g / L, 0.050g / L, 0.080g / L, 0.1g / L, 0.3g / L, 0.5g / L, 0.9g / L, 1.0g / L , 1.3g/L, etc.).
  • R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 and R 8 are each independently selected from a hydrogen atom, a substituted or substituted alkyl group, a substituted or substituted alkoxy group, A substituted or substituted carboxy group, a substituted or unsubstituted amino group, a substituted or unsubstituted alkyl fluorenyl group, a substituted or unsubstituted alkyl hydroxy group, preferably a hydrogen atom.
  • the crystallizing agent comprises 1,2-cyclohexanedicarboxylic acid, 1,2-cyclohexanedicarboxylate, a derivative of 1,2-cyclohexanedicarboxylic acid, 1,2-cyclohexane Any one or a combination of at least two of a derivative of an alkyl dicarboxylate, a derivative of 1,2-cyclohexanedicarboxylic anhydride, and 1,2-cyclohexanedicarboxylic anhydride.
  • Another object of the present invention is to provide a use of a crystallizing agent as one of the objects, which is used as a crystallizing agent in the process of preparing ⁇ -type high-strength gypsum.
  • the crystallizing agent is used as a crystallizing agent for preparing ⁇ -type high-strength gypsum by hydrothermal method, a crystallizing agent for preparing ⁇ -type high-strength gypsum by semi-dry method, or a crystal-transforming agent for preparing ⁇ -type high-strength gypsum by autoclaving.
  • the crystallizer is used as a crystallizer in the process of preparing ⁇ -type high-strength gypsum, and is combined with any one or at least two of a water-soluble trivalent aluminum salt and a water-soluble ferric salt. Mixed use.
  • a water-soluble trivalent aluminum salt and/or a water-soluble trivalent iron salt can be combined with the crystallizing agent of the present invention to enhance the effect of crystal transformation.
  • the third object of the present invention is to provide a method for preparing ⁇ -type high-strength gypsum, and the preparation method comprises the following steps:
  • step (4) is carried out: after the filter residue is dried, an ⁇ -type high-strength gypsum powder is obtained.
  • the ⁇ -type high-strength gypsum powder can also be subjected to grinding treatment as needed to improve the particle matching of the ⁇ -type high-strength gypsum powder.
  • the crystallizing agent according to one of the objects of the invention is used for the crystallizing preparation of ⁇ -type high-strength gypsum, and is capable of generating a high intensity of -1084 kJ/mol on the (114) surface of the ⁇ -CaSO 4 ⁇ 0.5H 2 O crystal.
  • Adsorption, in the process of gypsum crystallizing can produce gypsum crystals with a length to diameter ratio of about 1:1, and obtain high-strength ⁇ -type gypsum.
  • one of the purposes of the crystallizer is added in an amount of 0.01 to 0.2 wt%, such as 0.02 wt%, 0.04 wt%, 0.05 wt%, 0.07 wt%, of the mass of water. 0.09 wt%, 0.11 wt%, 0.15 wt%, and the like.
  • the mixing ratio of the crystallizer solution and gypsum is ⁇ 6:10, for example, 0.3:10, 0.8:10, 1:10, 2:10, 3:10, 4:10, etc.; preferably 0.1 to 5: 10.
  • the crystallizer solution is added with any one or a combination of at least two of a water-soluble trivalent aluminum salt and a water-soluble ferric iron salt.
  • the water-soluble trivalent aluminum salt comprises any one or a combination of at least two of aluminum chloride, aluminum sulfate, and aluminum nitrate.
  • the water-soluble ferric salt includes any one or a combination of at least two of ferric chloride, iron sulfate, and ferric nitrate.
  • the sum of the water-soluble trivalent aluminum salt and the water-soluble ferric salt is added in an amount of 0.03% or less, such as 0.02%, 0.01%, or the like.
  • the crystal transformation temperature is 110 to 140 ° C (for example, 115 ° C, 120 ° C, 125 ° C, 130 ° C, 135 ° C, etc.), and the menstrual time is 50 to 180 min (for example, 55 min, 65 min, 80 min, 100 min, 110 min). , 130min, 145min, 158min, 165min, 175min, etc.).
  • the alpha type high strength gypsum has a free water content of 7 to 15 wt% (e.g., 8 wt%, 9 wt%, 10 wt%, 11 wt%, 12 wt%, 13 wt%, 14 wt%, etc.).
  • the ⁇ -type high-strength gypsum powder has a free water content of ⁇ 0.7 wt%, such as 0.6 wt%, 0.5 wt%, 0.4 wt%, 0.3 wt%, 0.2 wt%, 0.1 wt%, and the like.
  • the gypsum to be crystallized in the present invention is not particularly limited, and any natural gypsum can be used in the present invention.
  • the gypsum to be crystallized of the present invention may be selected from the natural gypsum of GB/T5483-2008, preferably the special grade gypsum of GB/T5483-2008, the first grade natural gypsum, and the second grade natural gypsum.
  • the fourth object of the present invention is to provide an ⁇ -type high-strength gypsum prepared by the method described in the third object.
  • the ⁇ -type high-strength gypsum meets the performance requirements of the standard JC/T2038-2010 ⁇ -type high-strength gypsum.
  • the ⁇ -type high-strength gypsum has an average aspect ratio of 1:0.5 to 1:3.
  • the ⁇ -type high-strength gypsum has a 2-hour bending strength of ⁇ 5.0 MPa, for example, 6.0 MPa, 7.0 MPa, 8.0 MPa, 9.0 MPa, and the like.
  • the ⁇ -type high-strength gypsum has a compressive strength of ⁇ 43 MPa, for example, 44 MPa, 46 MPa, 48 MPa, 52 MPa, 55 MPa, 60 MPa, and the like.
  • the present invention has the following beneficial effects:
  • the ⁇ -type high-strength gypsum prepared by using the crystal-transforming agent of the present invention has a crystal length-to-diameter ratio in the range of 0.5 to 3.2:1, and has a 2-hour bending strength of 5.0 MPa or more and a drying pressure resistance of 43 MPa or more. strength.
  • succinic acid and glutaric acid can be used as a crystallizer for the production of ⁇ -type high-strength gypsum; 1,2-cyclohexanedicarboxylic acid in the (114) side of ⁇ -CaSO 4 ⁇ 0.5H 2 O crystal
  • the adsorption energy is as high as -1084KJ/mol, and the absolute value of the adsorption energy is much larger than that of succinic acid and glutaric acid.
  • 1,2-cyclohexanedicarboxylic acid and organic substances which are easily hydrolyzed in aqueous solution to form 1,2-cyclohexanedicarboxylic acid and 1,2-cyclohexanedicarboxylate They are all high-efficiency ⁇ -type high-strength gypsum crystallizers.
  • a method for preparing ⁇ -type high-strength gypsum comprising the following steps:
  • Pulping a crystallizer, trivalent aluminum (or ferric iron) and water are mixed to obtain a crystallizer solution, and then gypsum (calcium sulfate content: 85 wt%) is added to the crystallizer solution, and mixed. a gypsum suspension; the gypsum is added in an amount of 0.5 times that of the crystallizer solution;
  • step (2) is: the gypsum suspension is heated to 140 ° C, and the temperature is kept for 50 minutes for crystal transformation; after the completion of the crystal transformation, the gypsum slurry is sent to the next section through the bottom heat preservation discharge valve. Solid-liquid separation process.
  • step (2) is: the gypsum suspension is heated to 115 ° C, and the temperature is maintained for 180 minutes for crystal transformation; after the completion of the crystal transformation, the gypsum slurry is sent to the next section through the bottom heat preservation discharge valve. Solid-liquid separation process.
  • Example 3 The difference from Example 3 is that the gypsum content in the gypsum in the step (1) is 90% by weight.
  • Example 3 The difference from Example 3 is that the gypsum content in the gypsum in the step (1) is 80% by weight.
  • Example 3 The difference from Example 3 is that the crystallizing agent 1,2-cyclohexanedicarboxylic acid of the step (1) is replaced with glutaric acid, and the concentration of glutaric acid in the crystallizing agent solution is 1 g/L.
  • Example 3 The difference from Example 3 is that the crystallizing agent 1,2-cyclohexanedicarboxylic acid of the step (1) is replaced with glutaric acid, and the concentration of glutaric acid in the crystallizing agent solution is 1.5 g/L.
  • Example 3 The difference from Example 3 is that the crystallizing agent 1,2-cyclohexanedicarboxylic acid of the step (1) is replaced with potassium lauryl sulfate, and the concentration of potassium lauryl sulfate in the crystallizing agent solution is 1 g/ L.
  • Example 2 1:1 5.0 43.0
  • Example 3 2.5:1 6.8 65.0
  • Example 4 2:1 7.8 80.0
  • Example 5 3:1 7.1 61.0
  • Example 6 3:1 6.3 54.0
  • Example 7 0.5:1 6.2 52.0
  • Example 8 3.2:1 5.8 65.0
  • Example 9 2.5:1 6.8 70.0
  • Example 10 2.5:1 6.3 62.0
  • Example 11 2.5:1 6.9 70.0
  • Example 12 2.5:1 7.0 67.0
  • Example 13 2.5:1 6.7 60.0 Comparative example 1 3.8:1 4.0 40.0 Comparative example 2 4.5:1 4.2 38.0 Comparative example 3 50:1 0.4 1.0
  • the aspect ratio of the ⁇ -type high-strength gypsum crystal formed by gypsum crystal transformation is about 4:1, further increasing.
  • the concentration of the crystallizer does not reduce the aspect ratio of the ⁇ -type high-strength gypsum crystals formed by the crystal transformation; when the crystal conversion agent provided by the present invention is used, the crystal conversion agent having a concentration of 0.60 g/L can be naturally
  • the aspect ratio of ⁇ -type high-strength gypsum crystal prepared from gypsum as raw material is reduced to about 1:1.
  • the short columnar ⁇ -type high-strength gypsum crystal with a length to diameter ratio of about 1:1 is of great benefit for the production of high-strength ⁇ -type high-strength gypsum. Its 2-hour flexural strength is above 5.0 MPa, and the drying compressive strength is above 43.0 MPa. .
  • the present invention illustrates the process of the present invention by the above-described embodiments, but the present invention is not limited to the above process steps, that is, it does not mean that the present invention must rely on the above process steps to be implemented. It will be apparent to those skilled in the art that any modifications of the present invention, equivalent substitutions of the materials selected for the present invention, and the addition of the auxiliary ingredients, the selection of the specific means, etc., are all within the scope of the present invention.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

L'invention concerne un modificateur cristallin, qui est l'un quelconque ou une combinaison d'au moins deux parmi un composé ayant une structure de formule (I), un sel du composé ayant la structure de formule (I) et un composé ayant une structure de formule (II), dans lesquelles R1, R2, R3, R4, R5, R6, R7 et R8 sont chacun indépendamment choisis parmi des groupes organiques, R' représente un groupe méthyle, et n représente 0 ou 1. Le modificateur cristallin comprend deux groupes carboxyliques comme une pince dans l'eau, et peut produire une forte adsorption sur une surface (114) d'un cristal alpha-CaSO4•0,5H2O. Un gypse de résistance élevée de type alpha préparé par le modificateur cristallin présente un rapport longueur-diamètre de cristal dans la plage de 1:0,5 à 1:3, une résistance à la rupture en 2 heures supérieure à 5,0 MPa, et une résistance à la compression de séchage supérieure à 43 MPa.
PCT/CN2018/077418 2018-02-27 2018-02-27 Modificateur cristallin et son utilisation pour la préparation de gypse de résistance élevée de type alpha WO2019165578A1 (fr)

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CN201880003981.1A CN110023244B (zh) 2018-02-27 2018-02-27 一种转晶剂以及使用其制备α型高强石膏的用途
PCT/CN2018/077418 WO2019165578A1 (fr) 2018-02-27 2018-02-27 Modificateur cristallin et son utilisation pour la préparation de gypse de résistance élevée de type alpha

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CN111533475B (zh) * 2020-05-01 2022-06-14 厦门诺维特环保科技有限公司 一种转晶剂及利用该转晶剂制备α-型高强半水石膏的方法

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CN106044826A (zh) * 2016-05-26 2016-10-26 东南大学 一种用于生产α型高强石膏的转晶剂
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