CN117865183A - Clean production process for improving crystallinity granularity of re-ash - Google Patents
Clean production process for improving crystallinity granularity of re-ash Download PDFInfo
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- CN117865183A CN117865183A CN202410266785.0A CN202410266785A CN117865183A CN 117865183 A CN117865183 A CN 117865183A CN 202410266785 A CN202410266785 A CN 202410266785A CN 117865183 A CN117865183 A CN 117865183A
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- ash
- granularity
- production process
- crystallinity
- heavy ash
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 36
- 239000003513 alkali Substances 0.000 claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000012452 mother liquor Substances 0.000 claims abstract description 36
- 238000002425 crystallisation Methods 0.000 claims abstract description 30
- 230000008025 crystallization Effects 0.000 claims abstract description 30
- 239000003223 protective agent Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000010413 mother solution Substances 0.000 claims abstract description 8
- 239000002956 ash Substances 0.000 claims abstract 25
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 48
- 238000006703 hydration reaction Methods 0.000 claims description 43
- 230000036571 hydration Effects 0.000 claims description 39
- 239000007790 solid phase Substances 0.000 claims description 20
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000003054 catalyst Substances 0.000 claims description 15
- 239000003999 initiator Substances 0.000 claims description 15
- 239000007791 liquid phase Substances 0.000 claims description 13
- 239000002202 Polyethylene glycol Substances 0.000 claims description 11
- 229920001223 polyethylene glycol Polymers 0.000 claims description 11
- RZXLPPRPEOUENN-UHFFFAOYSA-N Chlorfenson Chemical compound C1=CC(Cl)=CC=C1OS(=O)(=O)C1=CC=C(Cl)C=C1 RZXLPPRPEOUENN-UHFFFAOYSA-N 0.000 claims description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 229920001897 terpolymer Polymers 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- -1 dicyclopentadienyl dimethyl titanium Chemical compound 0.000 claims description 7
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 150000004682 monohydrates Chemical class 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 4
- QCEOZLISXJGWSW-UHFFFAOYSA-K 1,2,3,4,5-pentamethylcyclopentane;trichlorotitanium Chemical compound [Cl-].[Cl-].[Cl-].CC1=C(C)C(C)([Ti+3])C(C)=C1C QCEOZLISXJGWSW-UHFFFAOYSA-K 0.000 claims description 3
- XSZYESUNPWGWFQ-UHFFFAOYSA-N 1-(2-hydroperoxypropan-2-yl)-4-methylcyclohexane Chemical compound CC1CCC(C(C)(C)OO)CC1 XSZYESUNPWGWFQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 2
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
- 238000001354 calcination Methods 0.000 abstract description 5
- MQRJBSHKWOFOGF-UHFFFAOYSA-L disodium;carbonate;hydrate Chemical compound O.[Na+].[Na+].[O-]C([O-])=O MQRJBSHKWOFOGF-UHFFFAOYSA-L 0.000 abstract description 5
- 239000006260 foam Substances 0.000 abstract description 4
- 230000037390 scarring Effects 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 3
- 238000002485 combustion reaction Methods 0.000 abstract description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 abstract 4
- 235000002918 Fraxinus excelsior Nutrition 0.000 abstract 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 abstract 2
- 235000017557 sodium bicarbonate Nutrition 0.000 abstract 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 abstract 1
- 235000017550 sodium carbonate Nutrition 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 11
- 229940001593 sodium carbonate Drugs 0.000 description 11
- 239000002245 particle Substances 0.000 description 5
- 239000002585 base Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229940076133 sodium carbonate monohydrate Drugs 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 206010039509 Scab Diseases 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- TXCDCPKCNAJMEE-UHFFFAOYSA-N dibenzofuran Chemical compound C1=CC=C2C3=CC=CC=C3OC2=C1 TXCDCPKCNAJMEE-UHFFFAOYSA-N 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000010587 phase diagram Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/22—Purification
- C01D7/24—Crystallisation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/22—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a clean production process for improving the crystallinity granularity of heavy ashes, belonging to the technical field of heavy ashes production. The invention connects the common heavy ash production system and the high-quality heavy ash production system in series, and utilizes the mother solution with high concentration and high temperature of the high-quality heavy ash to produce the common heavy ash, thereby realizing the high-efficiency utilization of the high-quality heavy ash mother solution; the method sends the return alkali into the heavy ash calciner to be calcined together with the sodium bicarbonate, so that the moisture of the wet sodium bicarbonate can be reduced, the scarring of the calciner is prevented, the common heavy ash sodium bicarbonate has larger and more uniform crystal granularity and lower water content on the premise of ensuring the yield, the steam consumption of the calcination process is reduced, and economic benefits are generated; the crystallization protective agent prepared by the invention has better wettability, solubility and wettability, can reduce the water content and salt content of monohydrate sodium carbonate, improve combustion efficiency, reduce steam consumption, reduce the water content and salt content of a product, prevent caking and scarring, stabilize foam in mother liquor, reduce foam generation and lighten expansion of the mother liquor.
Description
Technical Field
The invention belongs to the technical field of heavy ash production, and particularly relates to a clean production process for improving the crystallinity granularity of heavy ash.
Background
The sodium carbonate has the reputation of 'chemical industry master', plays a role in economic development, and can be applied to industries such as textile, detergent, glass, papermaking, metallurgy, chemical industry and the like in industry. Soda ash is classified into light soda ash (light ash) and heavy soda ash (heavy ash) according to the difference of bulk density, particle size and shape and stacking angle. The light ash is hydrated to form sodium carbonate monohydrate, the lattice structure of sodium carbonate is changed in the reaction process, and then the sodium carbonate monohydrate is calcined to decompose the combined water to obtain heavy ash, and the sodium carbonate monohydrate is calcined to avoid damaging the lattice arrangement structure of the sodium carbonate monohydrate, so that the heavy ash has the characteristics of low impurity content, large particle density and small stacking angle. With technological development and product demand, the production of heavy ash becomes the mainstream of product demand. The heavy ash is produced by a hydration method, which can be divided into a solid phase hydration method and a liquid phase hydration method, and the solid phase hydration method has simple equipment and simple operation and is mainly used for producing common heavy ash, and the granularity and uniformity of the product are not as good as those of the liquid phase hydration method. The heavy ash obtained by the liquid phase hydration method has low salt content and uniform granularity, and has a plurality of advantages. However, in the process of producing low-salt high-quality heavy ash by using a liquid phase hydration method, the salt brought by the light sodium carbonate is balanced by a method of discharging part of liquid phase hydration mother liquor, and the liquid phase hydration mother liquor has excessive problems in actual production, and if the liquid phase hydration mother liquor cannot be utilized, great resource waste and environmental pollution are generated. The liquid phase hydration mother liquor is reused to produce common heavy ash products with qualified quality indexes, meanwhile, the scab phenomenon of equipment in the production process is reduced, the steam consumption is reduced, and the production method is a difficult point of heavy ash production at present.
Disclosure of Invention
Aiming at the situation, in order to overcome the defect that the liquid phase hydration mother liquor cannot be reasonably recycled in the existing production process, the invention recycles the liquid phase hydration mother liquor to produce the common heavy ash product with larger and more uniform grain size and lower water content, and simultaneously reduces the scarring phenomenon of equipment in the production process and the steam consumption.
In order to achieve the above purpose, the following technical scheme is adopted: the invention provides a clean production process for improving the granularity of the crystallinity of re-ash, which comprises the following steps:
(1) Liquid phase hydration mother liquor in a high-quality heavy ash mother liquor barrel is pumped into a chemical water tank through a mother liquor pump, and the concentration of sodium carbonate in the mother liquor is adjusted by adding desalted water to obtain mother liquor I;
(2) The mother liquor I is sent into a solid-phase hydration machine through a compound water pump, meanwhile, light ash is sent into the solid-phase hydration machine through a light ash scraper and a feeding screw, then a crystallization protective agent is added for hydration reaction, and a sodium carbonate is obtained through centrifugal separation;
(3) Feeding the aqueous alkali generated by the reaction in the step (2) into a heavy ash calciner through an aqueous alkali screw, and feeding the return alkali into the heavy ash calciner through a return alkali scraper;
(4) And (3) sending the calcined product in the step (3) into an alkali cooling machine by a finished product scraper, cooling to room temperature, and sending into a screening system to obtain a common heavy ash product.
Further, the preparation of the crystallization protective agent comprises the following steps:
I. reacting dibenzofuran-2-methyl formate, acrylic acid-acrylic ester-sulfonate terpolymer, disuccinic acid polyethylene glycol, deionized water and a catalyst at 40-50 ℃ for 1-2h, and then adding 1mol/L sodium hydroxide solution to adjust the pH value to be 8-9;
II. Heating to 75-95 ℃ in nitrogen atmosphere, dropwise adding an initiator, continuing to react for 2-4h, filtering after the reaction is finished, and drying at 60 ℃ to obtain the crystallization protective agent.
Further, the concentration of the sodium carbonate in the mother liquor I after adjustment is 40-60tt.
Further, the mass ratio of the mother liquor I to the light ash to the crystallization protective agent is as follows: 80-100:10-15:0.015-0.02.
Further, the pressure of the solid phase hydration machine is-150-100 Pa, and the hydration outlet temperature of the solid phase hydration machine is 80-95 ℃.
Further, the mass ratio of the monohydrate alkali to the return alkali in the step (3) is 100-105:55-60.
Further, the furnace end pressure of the heavy ash calciner is-100-50 kPa, and the alkali outlet temperature of the heavy ash calciner is 160-200 ℃.
Further, the crystallization protective agent comprises the following components in parts by weight: 40-60 parts of dibenzofuran-2-methyl formate, 25-45 parts of acrylic acid-acrylic ester-sulfonate terpolymer, 5-15 parts of disuccinate polyethylene glycol, 50-60 parts of deionized water, 0.5-1 part of catalyst and 2.5-5 parts of initiator.
Further, the catalyst is one of dicyclopentadienyl dimethyl titanium, pentamethyl cyclopentadienyl titanium trichloride and dimethylsilyl tert-butylamine tetramethyl cyclopentadiene titanium dichloride.
Further, the initiator is one of azobisisobutyronitrile, tert-butyl peroxide, potassium persulfate, sodium persulfate and p-menthane hydroperoxide.
The beneficial effects of the invention are as follows:
(1) The invention connects the common heavy ash production system and the high-quality heavy ash production system in series, utilizes the high-concentration and high-temperature mother liquor of the high-quality heavy ash to produce the common heavy ash, realizes the high-efficiency utilization of the high-quality heavy ash mother liquor, and prevents the resource waste and the environmental pollution caused by the unreasonable utilization of the high-quality heavy ash mother liquor;
(2) The method has the advantages that the return alkali is also sent into the heavy ash calciner to be calcined together with the alkali, so that the moisture of wet alkali can be reduced, the alkali can be prevented from scarring in the calciner, the common heavy ash alkali has larger and more uniform crystal granularity and lower water content on the premise of ensuring the yield, the calcining capability is improved, the steam consumption of the calcining process is reduced, and huge economic benefits can be generated;
(3) According to the crystallization protective agent prepared by the invention, the dibenzofuran can improve the hydrophobicity and alkali resistance of a hydrophobic chain segment, the hydrophilic chain segment is increased by connecting the chain segment with the disuccinic acid polyethylene glycol, the dissolution performance and the surface activity of the crystallization protective agent are promoted, so that the crystallization protective agent has better wetting ability, the addition of the sulfonic acid group further promotes the solubility and the wettability of the crystallization protective agent, and water molecules are more effectively removed, so that the water content and the salt content of a water base are reduced, the combustion efficiency of a calciner is improved, the steam consumption is reduced, the water content and the salt content crystallization of a common heavy ash product are reduced, the adhesion force between the water base particles can be reduced, the agglomeration of the water base and the common heavy ash product in the storage and transportation processes is effectively prevented, the scabbing of the water base and the common heavy ash product in a solid-phase hydration machine and a heavy ash calciner is prevented, the foam in a mother solution is stabilized, the generation of the foam is reduced, and the expansion phenomenon of the mother solution is lightened.
Drawings
FIG. 1 is a flow chart of a clean production process for improving the crystallinity granularity of the re-ash according to the present invention;
FIG. 2 is H 2 O-Na 2 CO 3 A system phase diagram;
FIG. 3 is a bar graph of the ratio of screen residue to 180 μm for each of the examples and comparative examples of the present invention;
FIG. 4 is a bar graph of the screen reject ratio of not less than 2mm for each of the examples and comparative examples of the present invention.
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention.
Legend: 1. a high-quality heavy ash mother liquor barrel; 2. a mother liquid pump; 3. a combination water tank; 4. a compound water pump; 5. a solid phase hydration machine; 6. a light ash scraper; 7. a feed screw; 8. a water alkali screw; 9. a heavy ash calciner; 10. an alkali returning scraper; 11. a finished product scraper; 12. an alkali cooling machine; 13. and a screening system.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by those skilled in the art based on the embodiments of the present invention without making any inventive effort are within the scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the present invention. The preferred methods and materials described herein are illustrative only and should not be construed as limiting the scope of the present application.
The experimental methods in the following examples are conventional methods unless otherwise specified, and the experimental materials used in the following examples are commercially available unless otherwise specified.
The hydration reaction conditions according to the invention are described with reference to FIG. 2, H 2 O-Na 2 CO 3 And (5) a system phase diagram.
Example 1
Clean production process for improving crystallinity granularity of re-ash
According to fig. 1, the production process comprises the following steps:
(1) Liquid phase hydration mother liquor in a high-quality heavy ash mother liquor barrel is pumped into a chemical water tank through a mother liquor pump, and the concentration of sodium carbonate in the mother liquor is adjusted by adding desalted water to obtain mother liquor I;
(2) The mother liquor I is sent into a solid-phase hydration machine through a compound water pump, meanwhile, light ash is sent into the solid-phase hydration machine through a light ash scraper and a feeding screw, then a crystallization protective agent is added for hydration reaction, and a sodium carbonate is obtained through centrifugal separation;
(3) Feeding the aqueous alkali generated by the reaction in the step (2) into a heavy ash calciner through an aqueous alkali screw, and feeding the return alkali into the heavy ash calciner through a return alkali scraper;
(4) And (3) sending the calcined product in the step (3) into an alkali cooling machine by a finished product scraper, cooling to room temperature, and sending into a screening system to obtain a common heavy ash product.
The preparation of the crystallization protective agent comprises the following steps:
I. reacting dibenzofuran-2-methyl formate, acrylic acid-acrylic ester-sulfonate terpolymer, disuccinic acid polyethylene glycol, deionized water and a catalyst at 40 ℃ for 1h, and then adding 1mol/L sodium hydroxide solution to adjust the pH value to be 8-9;
II. Heating to 75 ℃ in nitrogen atmosphere, dropwise adding an initiator, continuing to react for 2 hours, filtering after the reaction is finished, and drying at 60 ℃ to obtain the crystallization protective agent.
The concentration of the sodium carbonate in the mother liquor I after adjustment is 40tt.
The mass ratio of the mother solution I to the light ash to the crystallization protective agent is as follows: 80:10:0.015.
the pressure of the solid phase hydration machine is-150-100 Pa, and the hydration outlet temperature of the solid phase hydration machine is 80 ℃.
The mass ratio of the monohydrate alkali to the return alkali in the step (3) is 100:55.
the furnace end pressure of the heavy ash calciner is-100 kPa, and the alkali outlet temperature of the heavy ash calciner is 160 ℃.
The crystallization protective agent comprises the following components in parts by weight: 40 parts of dibenzofuran-2-methyl formate, 25 parts of acrylic acid-acrylic ester-sulfonate terpolymer, 5 parts of disuccinate polyethylene glycol, 50 parts of deionized water, 0.5 part of catalyst and 2.5 parts of initiator.
The catalyst is dicyclopentadienyl dimethyl titanium.
The initiator is azobisisobutyronitrile.
Example 2
Clean production process for improving crystallinity granularity of re-ash
The production process includes the same steps as in example 1.
The preparation of the crystallization protective agent comprises the following steps:
I. reacting dibenzofuran-2-methyl formate, acrylic acid-acrylic ester-sulfonate terpolymer, disuccinic acid polyethylene glycol, deionized water and a catalyst at 50 ℃ for 2 hours, and then adding 1mol/L sodium hydroxide solution to adjust the pH value to be 8-9;
II. Heating to 95 ℃ in nitrogen atmosphere, dropwise adding an initiator, continuing to react for 4 hours, filtering after the reaction is finished, and drying at 60 ℃ to obtain the crystallization protective agent.
The concentration of the sodium carbonate in the mother liquor I after adjustment is 60tt.
The mass ratio of the mother solution I to the light ash to the crystallization protective agent is as follows: 100:15:0.02.
the pressure of the solid phase hydration machine is 100Pa, and the hydration outlet temperature of the solid phase hydration machine is 95 ℃.
The mass ratio of the monohydrate alkali to the return alkali in the step (3) is 105:60.
the furnace end pressure of the heavy ash calciner is 50kPa, and the alkali outlet temperature of the heavy ash calciner is 200 ℃.
The crystallization protective agent comprises the following components in parts by weight: 60 parts of dibenzofuran-2-methyl formate, 45 parts of acrylic acid-acrylic ester-sulfonate terpolymer, 15 parts of disuccinate polyethylene glycol, 60 parts of deionized water, 01 parts of catalyst and 5 parts of initiator.
The catalyst is pentamethyl cyclopentadienyl titanium trichloride.
The initiator is tert-butyl peroxy alcohol.
Example 3
Clean production process for improving crystallinity granularity of re-ash
The production process includes the same steps as in example 1.
The preparation of the crystallization protective agent comprises the following steps:
I. reacting dibenzofuran-2-methyl formate, acrylic acid-acrylic ester-sulfonate terpolymer, disuccinic acid polyethylene glycol, deionized water and a catalyst at 45 ℃ for 1.5 hours, and then adding 1mol/L sodium hydroxide solution to adjust the pH value to be 8-9;
II. Heating to 80 ℃ in nitrogen atmosphere, dropwise adding an initiator, continuing to react for 2.5 hours, filtering after the reaction is finished, and drying at 60 ℃ to obtain the crystallization protective agent.
The concentration of the sodium carbonate in the mother liquor I after adjustment is 50tt.
The mass ratio of the mother solution I to the light ash to the crystallization protective agent is as follows: 90:12:0.018.
the pressure of the solid phase hydration machine is 50Pa, and the hydration outlet temperature of the solid phase hydration machine is 90 ℃.
The mass ratio of the monohydrate alkali to the return alkali in the step (3) is 102:58.
the furnace end pressure of the heavy ash calciner is 0kPa, and the alkali outlet temperature of the heavy ash calciner is 180 ℃.
The crystallization protective agent comprises the following components in parts by weight: 50 parts of dibenzofuran-2-methyl formate, 30 parts of acrylic acid-acrylic ester-sulfonate terpolymer, 10 parts of disuccinate polyethylene glycol, 55 parts of deionized water, 0.7 part of catalyst and 3.5 parts of initiator.
The catalyst is silyl tert-butylamine tetramethyl cyclopentadiene titanium dichloride.
The initiator is p-menthane hydroperoxide.
Comparative example 1
Clean production process for improving crystallinity granularity of re-ash
This comparative example is different from example 1 in that the crystallization protectant is not used in the step (2), and the remaining components, component contents, and preparation process include the same steps as those of example 1.
Analysis of results
Each index of the common heavy ash products produced in examples 1 to 3 and comparative example 1 was examined, and the examination results are shown in Table 1.
TABLE 1 results of measurement of various indexes of the ordinary heavy gray products produced in examples 1-3 and comparative example 1
| Index name | Index requirements | Example 1 | Example 2 | Example 3 | Comparative example 1 |
| Total alkali content (dry basis Na 2 CO 3 Meter (C) | ≥99.4% | 99.75% | 99.62% | 99.78% | 98.72% |
| Total alkali content (in wet basis Na 2 CO 3 Meter (C) | ≥98.1% | 99.22% | 99.15% | 99.20% | 98.28% |
| Sodium chloride% | ≤0.3% | 0.12% | 0.15% | 0.13% | 0.23% |
| Iron% | ≤0.003% | 0.0017% | 0.0016% | 0.0015% | 0.0022% |
| Water insoluble matter% | ≤0.02% | 0.010% | 0.012% | 0.009% | 0.011% |
| Sulfate% | ≤0.02% | 0.012% | 0.008% | 0.011% | 0.018% |
| Calcium% | ≤0.03% | 0.019% | 0.021% | 0.018% | 0.026% |
| Arsenic% | ≤0.0001% | 0.00006% | 0.00005% | 0.00004% | 0.0001% |
| Heavy metal (Pb)% | ≤0.0005% | 0.0002% | 0.0002% | 0.0003% | 0.0004% |
| Alkali monohydrate water content% | ≤14.5% | 10.8% | 9.8% | 10.5% | 13.2% |
| t/t alkali (steam consumption) | - | 0.386 | 0.390 | 0.391 | 0.425 |
The screen residue ratio of the particle size of 180 μm or more and the screen residue ratio of the particle size of 2mm or more were measured in each of the examples and comparative examples of the present invention, and the measurement results are shown in FIG. 3 and FIG. 4, respectively.
As shown in Table 1, each index of the prepared common heavy ash product meets the index requirement and is superior to that of the comparative example, the common heavy ash product prepared under the process conditions of the invention has high total alkali content, low salt content, less impurity content and low water content, the calcining capability is improved, the steam consumption of the calcining process is reduced, and huge economic benefits can be produced, as shown in FIG. 3 and FIG. 4, the ratio of the screen residue with the granularity of more than or equal to 180 mu m of the common heavy ash product prepared by the invention is larger than that of the comparative example, the ratio of the screen residue with the granularity of more than or equal to 2mm is smaller than that of the comparative example, and the crystal granularity of the common heavy ash product produced by the invention is larger and more uniform.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
The invention and its embodiments have been described above with no limitation, and the invention is illustrated in the figures of the accompanying drawings as one of its embodiments, without limitation in practice. In summary, those skilled in the art, having benefit of this disclosure, will appreciate that the invention can be practiced without the specific details disclosed herein.
Claims (10)
1. A clean production process for improving the crystallinity granularity of re-ash is characterized by comprising the following steps: the method comprises the following steps:
(1) Liquid phase hydration mother liquor in a high-quality heavy ash mother liquor barrel is sent into a chemical combination water tank through mother liquor, and the concentration of mother liquor sodium carbonate is adjusted by adding desalted water to obtain mother liquor I;
(2) The mother liquor I is sent into a solid-phase hydration machine through a compound water pump, meanwhile, light ash is sent into the solid-phase hydration machine through a light ash scraper and a feeding screw, then a crystallization protective agent is added for hydration reaction, and a sodium carbonate is obtained through centrifugal separation;
(3) Feeding the aqueous alkali generated by the reaction in the step (2) into a heavy ash calciner through an aqueous alkali screw, and feeding the return alkali into the heavy ash calciner through a return alkali scraper;
(4) And (3) sending the calcined product in the step (3) into an alkali cooling machine by a finished product scraper, cooling to room temperature, and sending into a screening system to obtain a common heavy ash product.
2. The clean production process for improving the crystallinity granularity of the re-ashes according to claim 1, wherein: the preparation of the crystallization protective agent comprises the following steps:
I. reacting dibenzofuran-2-methyl formate, acrylic acid-acrylic ester-sulfonate terpolymer, disuccinic acid polyethylene glycol, deionized water and a catalyst at 40-50 ℃ for 1-2h, and then adding 1mol/L sodium hydroxide solution to adjust the pH value to be 8-9;
II. Heating to 75-95 ℃ in nitrogen atmosphere, dropwise adding an initiator, continuing to react for 2-4h, filtering after the reaction is finished, and drying at 60 ℃ to obtain the crystallization protective agent.
3. The clean production process for improving the crystallinity granularity of the re-ashes according to claim 2, wherein: the concentration of the sodium carbonate in the mother liquor I after adjustment is 40-60tt.
4. A clean production process for improving the crystallinity granularity of the re-ashes according to claim 3, wherein: the mass ratio of the mother solution I to the light ash to the crystallization protective agent is as follows: 80-100:10-15:0.015-0.02.
5. The clean production process for improving the crystallinity granularity of the re-ashes according to claim 4, wherein: the pressure of the solid phase hydration machine is-150-100 Pa, and the hydration outlet temperature of the solid phase hydration machine is 80-95 ℃.
6. The clean production process for improving the crystallinity granularity of the re-ashes according to claim 5, wherein: the mass ratio of the monohydrate alkali to the return alkali in the step (3) is 100-105:55-60.
7. The clean production process for improving the crystallinity granularity of the re-ashes according to claim 6, wherein: the furnace end pressure of the heavy ash calciner is-100-50 kPa, and the alkali outlet temperature of the heavy ash calciner is 160-200 ℃.
8. The clean production process for improving the crystallinity granularity of the re-ashes according to claim 7, wherein: the crystallization protective agent comprises the following components in parts by weight: 40-60 parts of dibenzofuran-2-methyl formate, 25-45 parts of acrylic acid-acrylic ester-sulfonate terpolymer, 5-15 parts of disuccinate polyethylene glycol, 50-60 parts of deionized water, 0.5-1 part of catalyst and 2.5-5 parts of initiator.
9. The clean production process for improving the crystallinity granularity of the re-ashes according to claim 8, wherein: the catalyst is one of dicyclopentadienyl dimethyl titanium, pentamethyl cyclopentadienyl titanium trichloride and dimethylsilyl tert-butylamine tetramethyl cyclopentadiene titanium dichloride.
10. The clean production process for improving the crystallinity granularity of the re-ashes according to claim 9, wherein: the initiator is one of azobisisobutyronitrile, tert-butyl peroxide, potassium persulfate, sodium persulfate and p-menthane hydroperoxide.
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