CN1202005C - Process for preparing calcium metaborate from borax and lime - Google Patents
Process for preparing calcium metaborate from borax and lime Download PDFInfo
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- CN1202005C CN1202005C CN 03128749 CN03128749A CN1202005C CN 1202005 C CN1202005 C CN 1202005C CN 03128749 CN03128749 CN 03128749 CN 03128749 A CN03128749 A CN 03128749A CN 1202005 C CN1202005 C CN 1202005C
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- borax
- lime
- calcium metaborate
- metaborate
- cooling
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- 229910021538 borax Inorganic materials 0.000 title claims abstract description 69
- 239000004328 sodium tetraborate Substances 0.000 title claims abstract description 68
- 235000010339 sodium tetraborate Nutrition 0.000 title claims abstract description 67
- ILOKQJWLMPPMQU-UHFFFAOYSA-N calcium;oxido(oxo)borane Chemical compound [Ca+2].[O-]B=O.[O-]B=O ILOKQJWLMPPMQU-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000004571 lime Substances 0.000 title claims description 26
- 235000008733 Citrus aurantifolia Nutrition 0.000 title claims description 23
- 235000011941 Tilia x europaea Nutrition 0.000 title claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000012452 mother liquor Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 239000000047 product Substances 0.000 claims abstract description 15
- 230000002308 calcification Effects 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 13
- 238000001704 evaporation Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- 230000008020 evaporation Effects 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 239000000292 calcium oxide Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 15
- 229910004835 Na2B4O7 Inorganic materials 0.000 claims description 11
- 239000012065 filter cake Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 9
- 239000011734 sodium Substances 0.000 claims description 8
- NVIFVTYDZMXWGX-UHFFFAOYSA-N sodium metaborate Chemical compound [Na+].[O-]B=O NVIFVTYDZMXWGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 6
- 239000000920 calcium hydroxide Substances 0.000 claims description 6
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 6
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 6
- 239000008267 milk Substances 0.000 claims description 6
- 210000004080 milk Anatomy 0.000 claims description 6
- 235000013336 milk Nutrition 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 4
- 230000005484 gravity Effects 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 2
- 150000004683 dihydrates Chemical class 0.000 claims description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims 4
- 239000001569 carbon dioxide Substances 0.000 claims 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims 2
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 claims 1
- 239000012141 concentrate Substances 0.000 claims 1
- 239000012527 feed solution Substances 0.000 claims 1
- 239000012535 impurity Substances 0.000 claims 1
- 238000004064 recycling Methods 0.000 claims 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052796 boron Inorganic materials 0.000 abstract description 8
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 abstract description 5
- 238000002425 crystallisation Methods 0.000 abstract description 5
- 230000008025 crystallization Effects 0.000 abstract description 5
- 159000000000 sodium salts Chemical class 0.000 abstract description 4
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 abstract description 3
- FVJFRFUSHCIRKP-UHFFFAOYSA-N disodium;hydrogen borate Chemical compound [Na+].[Na+].OB([O-])[O-] FVJFRFUSHCIRKP-UHFFFAOYSA-N 0.000 abstract 1
- 229910001607 magnesium mineral Inorganic materials 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 13
- -1 calcium metaborate tetrahydrate Chemical class 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- GTUNMKRGRHOANR-UHFFFAOYSA-N [B].[Ca] Chemical compound [B].[Ca] GTUNMKRGRHOANR-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000003763 carbonization Methods 0.000 description 5
- 235000017550 sodium carbonate Nutrition 0.000 description 5
- 238000003825 pressing Methods 0.000 description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 3
- 235000019738 Limestone Nutrition 0.000 description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 239000006028 limestone Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 229910003252 NaBO2 Inorganic materials 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 2
- 159000000007 calcium salts Chemical class 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 2
- 239000001095 magnesium carbonate Substances 0.000 description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- AJFXNBUVIBKWBT-UHFFFAOYSA-N disodium;boric acid;hydrogen borate Chemical compound [Na+].[Na+].OB(O)O.OB(O)O.OB(O)O.OB([O-])[O-] AJFXNBUVIBKWBT-UHFFFAOYSA-N 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 150000004685 tetrahydrates Chemical class 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
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- Processing Of Solid Wastes (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to a method for preparing calcium metaborate CaO. B2O3. nH2O (wherein n=2, 4 or 6) from borax and calcium oxide and a technical process for comprehensively utilizing byproducts. The method is composed of the steps of calcification, press filtration, drying, product generation, evaporation, carbonation, crystallization by cooling, centrifugal separation and processing in a borax workshop. Borax and calcium oxide are directly calcified under the pH larger than or equal to 11 and at the temperature lower than 45 DEG C for 3 to 16 hours, and products are filtered and dried. Filter liquor is evaporated, carbonated, crystallized by cooling and centrifugally separated to recover borax, and washing water and mother liquor containing a large amount of sodium carbonate and a small amount of disodium borate are used as raw material for preparing borax from boron and magnesium mineral. The present invention has the advantages of sufficiently and effectively utilizing sodium salt and borate and reducing the production cost and satisfies market requirements.
Description
The invention relates to the technical field of preparation of calcium metaborate CaO.B by borax and lime2O3·nH2O (wherein, n is 2, 4 or 6) and byproducts are comprehensively utilized.
Calcium metaborate does not occur in nature. The results of the previous study show that: "the complexity of synthesizing calcium metaborate is that it must be formed at a pH above 11; at such high pH, however, excess calcium is precipitated as calcium hydroxide, which generally reduces the purity of the calcium metaborate crystals. "therefore, the method of laboratory synthesis recommended in the literature is that of B2O3/Na2O-0.93-0.50 (i.e. a mixture of borax and sodium hydroxide) solution to precipitate calcium chloride solution, and the former must be in large excess (three times) than calcium chloride.
The industrial method for directly preparing calcium metaborate from borax is only a method for carrying out double decomposition reaction on borax, calcium salt and lime milk, wherein the calcium salt can be calcium chloride, calcium sulfate or calcium nitrate, and can also be a mixture of calcium oxide and corresponding acid. The proportion of the raw materials is strictly controlled, and the industrially applicable calcium metaborate can be prepared. The common disadvantage of these processes is that in order to obtain the desired product, the mother liquor contains a certain amount of borate in addition to sodium salt, and both salts are difficult to separate completely, which limits the application field and market price of the recovered sodium salt, and reduces the economic benefit of production.
The invention relates to a method for preparing calcium metaborate CaO&B from borax and lime2O3·nH2The technological process of O (where n is 2, 4 or 6) is that the raw materials of borax and lime (lime powder, slaked lime powder or lime milk) are directly mixed according to their mole ratio Na2B4O7·10H2Carrying out calcification reaction with the ratio of O to CaO being 1: 0.8-1.1, the pH value being more than or equal to 11, the temperature being lower than 45 ℃, the liquid-solid ratio being 2-8: 1, reacting for 3-16 hours under stirring, and filtering and drying the product to obtain a dihydrate or tetrahydrate product of calcium metaborate; evaporating the filtrate and carbonic acidMelting, cooling, crystallizing and centrifugally separating to recover borax; the mother liquor containing a large amount of sodium carbonate and disodium tetraborate and the washing water are used as raw materials for preparing borax from the ascharite, thereby realizing the full and effective comprehensive utilization of sodium and boron.
The invention is characterized by being realized according to the following reactions:
reacting with NaBO2To keep the pH value of the medium to be more than or equal to 11 under the alkaline condition and remove sodium brought by borax to obtain a byproduct NaBO2Subjecting the aqueous solution to a carbonation reaction:
converted to Na2B4O7Cooling with Na2B4O7·10H2The O form crystallizes out. After centrifugal separation, returning borax to prepare calcium metaborate; the mother liquor contains a large amount of Na2CO3And a small amount of Na2B4O7Sent to a workshop for manufacturing borax by taking ascharite as a raw material to be used as the raw material.
Therefore, the process is essentially to prepare calcium metaborate from the raw materials of the ascharite and the limestone, and the borax is only an intermediate product.
Description of the drawings the production process of calcium metaborate according to the invention can be seen in the description attached to fig. 1:
wherein: 1-calcification, 2-filter pressing, 3-drying, 4-product (calcium metaborate), 5-evaporation, 6-carbonation, 7-cooling crystallization, 8-centrifugal separation, 9-borax workshop, 10-clear water, 11-lime and 12-borax.
The lime raw material (11) used by the invention can be lime powder (CaO) or slaked lime powder Ca (OH) with qualified quality for chemical engineering2. The powder can be directly used, or the powder material and the boron-calcium washing water are mixed into slurry in a slurry mixing tank and pumped into a calcification tank by compressed gas or a pump. If it isIf the quality of lime is not ideal, a lime slaking machine can be arranged to remove undecomposed limestone and over-burnt lime blocks in the lime to prepare lime milk for use.
Thecalcification reaction tank (1) can be an open type tank or a tank with an end closure, but all tanks have a stirring device. Filling washing water and clear water in a calcification reaction tank according to the liquid-solid ratio of 2-8: 1, and adding Cao to Na according to the molar ratio of calcification reaction materials2O4O7·1OH2Adding lime powder (11) (slaked lime powder or lime milk) and borax (12) into the mixture with O in the ratio of 0.8-1.1: 1 under stirring, and reacting at the temperature lower than 45 ℃ for 3-16 hours. Then the slurry in the calcification tank is sent to a plate-and-frame filter press (2) for filtering, the filter cake is washed by clear water to remove sodium metaborate, then the filter cake is sent to be dried, and the washing water is returned to the calcification ingredients. And (3) drying by adopting a rotary flash evaporation dryer or a fluidized bed dryer or a hollow blade stirring dryer, wherein the drying temperature is more than or equal to 105 ℃ when the calcium metaborate tetrahydrate is prepared, and the temperature is more than or equal to 120 ℃ when the calcium metaborate dihydrate is prepared. Specifically, the drying temperature and time can be controlled according to the requirements of users, and the product containing B can be produced2O334-35% of calcium metaborate tetrahydrate can also be used for producing the product containing B2O340-42% calcium metaborate dihydrate; the filtered calcification mother liquor is sent to an evaporator (5), dewatered, evaporated and concentrated to the specific gravity of 1.25-1.32, and then sent to a carbonating reactor (6), the sodium metaborate solution is carbonated by using the carbonation tail gas of a borax workshop (9), the temperature is 55-72 ℃, the pressure of the carbonation gas is 0.2-0.7Mpa, and the reaction is finished when the pH value of the solution is reduced to 9.0-10.2. The feed is then discharged to a cooling crystallizer (7) and cooled to 25-35 ℃. Borax is Na2O4O7·10H2Crystallizing in the form of O, centrifugally separating (8), washing away mother liquid carried in borax by using clear water, returning the obtained borax to a calcification tank to be used as a raw material, and sending filtrate to a borax workshop (9) to be used as the raw material. (300 kg of Na and 280 kg of sodium carbonate can be recovered from each ton of calcium metaborate dihydrate product2O4O7About 25 kg). The borax workshop takes ascharite, soda ash and limestone as raw materials, and adopts the traditional carbon-alkali method to manufacture borax.
The concentrated sodium metaborate solution can be used for CO in tail gas discharged by a carbon decomposition tank of a boron sand plant2For carbonation, the conditions are: pressure of 0.2-0.7Mpa, CO in gas2The concentration is more than 5 percent. The carbonation reactor may be a bubble column, a bubble column or a combination of both.
The mother liquor after borax removal and washing water are sent to a borax workshop (9) to be used as raw materials, a plurality of carbonization tanks with stirring and steam jacket heating are arranged in a borax device, roasted ludwigite ore powder and supplemented sodium carbonate solution are filled in the carbonization tanks, and kiln gas (containing CO) of a lime kiln is introduced230-36% of gas) under the pressure of 0.5MPa or more at the temperature of 125-135 ℃ to decompose the boron-containing mineral to generate soluble sodium borate salt, insoluble basic magnesium carbonate and magnesium carbonate, and the carbonized liquid is cooled by filter pressing to crystallize borax. The tail gas discharged from the carbon decomposition tank contains CO25-20% and the pressure is above 0.4MPa, and can be used for carbonating sodium metaborate solution.
The technological process realizes the full and effective comprehensive utilization of sodium salt and borate, reduces the production cost and is suitable for the market price.
Detailed Description
Example 1
Adding boron-calcium washing water 1.5m into a calcification reaction tank with a stirrer3Clear water 1.7m3Starting a stirrer, adding 158kg of chemical lime powder, and adding 1000kg of borax (containing 456kg of recycled borax) to react for 8 hours at normal temperature. After the reaction is finished, pumping the boron-calcium material to a plate-and-frame filter press by a slurry pump for filtering, wherein the feeding pressure is 0.4Mpa, enabling filtered mother liquor to automatically flow into calcium mother liquor, then adding the mother liquor into a double-effect evaporator by a feeding pump, controlling the specific gravity of final effect material liquor, and discharging the solution to a concentrated solution tank when the specific gravity of the final effect material liquor reaches 1.28. Adding the concentrated solution into a carbonization tower by a concentrated solution pump, adjusting the amount of cooling water to keep the temperature of the liquid at the bottom of the tower at 65 ℃, introducing the carbonized tail gas from a borax workshop, keeping the inlet pressure at 0.4Mpa, and carbonizingThe tail gas is sent into a tail gas tank to be used as a whole plant compressed gas source. When the pH value of the liquid at the bottom of the carbonization tower is reduced to below 9.8, the liquid at the bottom of the tower can be discharged to a borax cooling crystallization tank, a stirrer is started, cooling water is introduced to cool the liquid so as to crystallize the borax, and the liquid can be discharged when the temperature of the liquid is reduced to 30 ℃. Separating the crystallized slurry containing borax by centrifuge, washing mother liquor carried in borax with small amount of clear water to obtain 456kg of recovered borax, returning to calcification tank as raw material for preparing calcium metaborate, and collecting 736kg of borax mother liquor and washing water (containing Na) separated by centrifuge2CO3129kg，Na2B4O726kg) is sent to a borax workshop for batching, then boron ore powder and a small amount of soda ash are added, lime kiln gas is introduced for pressurized carbonization, and boron in the boron ore is converted into soluble Na2B4O7Cooling and crystallizing to obtain borax Na2B4O7·10H2O。
And washing off the entrained sodium metaborate solution from the calcium metaborate filter cake on the filter press by using clear water until the pH value of the washing water is less than 9, and then discharging. The washing water is completely returned to the ingredients. The wet filter cake is sent to a rotary flash evaporation dryer and dried by hot air with the temperature higher than 280 ℃, the dried finished product is calcium metaborate dihydrate, and the finished product contains B2O341.5％、CaO 35.1％、Na2O%<0.5%, weight 411.5 kg.
Example 2
Adding boron-calcium washing water 1.5m into a reaction tank with an open stirrer3Clear water 1.7m3Starting the stirrer, adding 213kg of slaked lime powder containing 71 percent of CaO, adding 1000kg of borax (containing 451kg of recycled borax), and reacting for 9 hours at normal temperature to finish the reaction. The slurry was pumped to a filter press by a pump. Filter pressing, filter cake washing, mother liquor evaporation concentration, sodium metaborate solution carbonation, borax crystallization cooling, borax centrifugal separation and the like are performed in the same operation process as the example I, so that 451kg of recovered borax is obtained, and 715kg of carbon alkaline solution (borax mother liquor and washing water) sent to a borax workshop contains Na2CO3129kg，Na2B4O722kg。
The washed calcium metaborate filter cake discharged from the filter press is sent to a rotary flash evaporation drier and dried by hot air with the temperature higher than 300 ℃ to obtain 427kg of finished product containing B2O341 percent, CaO 35.4 percent and Na2O＜0.5％。
Example 3
Adding boron-calcium washing water 1.5m into a reaction tank with an open stirrer3Clear water 0.8m3Starting the mixer, adding lime milk containing CaO 150g/L and 0.94m31000kg of borax (containing 450kg of recovered borax) was added, and the reaction was completed for 6 hours. The slurry was pumped to a filter press by a pump. Filter pressing, filter cake washing, mother liquor evaporation concentration, sodium metaborate solution carbonation, borax crystallization cooling, borax centrifugal separation and other operation processes are the same as the example I, 450kg of recovered borax is obtained, and boron is sent710kg of carbon alkali liquor (borax mother liquor and washing water) in sand workshop, wherein the carbon alkali liquor contains Na2CO3128kg，Na2B4O721.5kg。
The washed calcium metaborate filter cake discharged from the filter press is sent to a hollow paddle type stirring dryer, and is heated and dried by 0.5Mpa steam, the retention time of the materials is 1 hour, the discharging temperature is 120 ℃, and 422kg of finished products containing B is obtained2O341.6 percent of CaO, 33.4 percent of CaO and Na2O＜0.5％。
Claims (6)
1. A process for preparing calcium metaborate from borax and lime features that the raw materials of borax and lime are directly used and Na is proportionally mixed according to their mole ratio2B4O7·10H2The ratio of O to CaO is 1: 0.8-1.1, the pH value of the calcification reaction is more than or equal to 11, the temperature is lower than 45 ℃, the liquid-solid ratio is 2-8: 1, the reaction is carried out for 3-16 hours under stirring, and the product is filtered and dried to obtain the dihydrate product of the calcium metaborate; evaporating, carbonating, cooling, crystallizing, and centrifuging the filtrate to recover borax; mother liquor and washing water containing large amount of sodium carbonate and disodium tetraborateAs a raw material for producing borax from boresite.
2. The method for preparing calcium metaborate according to claim 1, wherein the raw material lime is lime powder or slaked lime powder or lime milk prepared by removing impurities; the powder material can be directly added or added into a reaction tank after being mixed into slurry.
3. The process for producing calcium metaborate according to claim 1, wherein the separation of the slurry for the calcification reaction is carried out by filtration using a plate and frame filter press, the filter cake is washed with clean water, and the washing water is returned to the calcification mixture.
4. The method for preparing calcium metaborate according to claim 1, wherein the drying process of calcium metaborate is performed byusing a spin flash dryer, a fluidized bed dryer or a hollow blade stirring dryer, wherein the drying temperature is 120-300 ℃.
5. The process for producing calcium metaborate according to claim 1, wherein after removing water from the filtrate by evaporation, the feed solution is carbonated by introducing carbon dioxide gas at a specific gravity of the concentrate of 1.25 to 1.30 to convert sodium metaborate into sodium tetraborate Na2B4O7And recycling sodium carbonate; the carbonation conditions were: the pressure of the carbonated gas is 0.2-0.7Mpa, the concentration of carbon dioxide is higher than 5%, the temperature is 55-70 ℃, and the pH value of the final feed liquid is 9.0-10.2.
6. A process for preparing calcium metaborate according to claim 1, in which the separation of sodium tetraborate from sodium carbonate is carried out by cooling, the sodium tetraborate being in the form of borax Na2B4O7·10H2Crystallizing out in the form of O, cooling to 25-35 deg.C, separating borax crystal from mother liquor with centrifuge, washing sodium carbonate in borax with clear water, and recovering borax as raw material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03128749 CN1202005C (en) | 2003-05-09 | 2003-05-09 | Process for preparing calcium metaborate from borax and lime |
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| CN 03128749 CN1202005C (en) | 2003-05-09 | 2003-05-09 | Process for preparing calcium metaborate from borax and lime |
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| CN1202005C true CN1202005C (en) | 2005-05-18 |
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| CN108301045B (en) * | 2018-03-15 | 2021-02-12 | 中国科学院新疆理化技术研究所 | Calcium metaborate birefringent crystal, preparation method and application thereof |
| CN112479221A (en) * | 2020-12-21 | 2021-03-12 | 河北昊德生物科技有限公司 | Production and synthesis process of sodium octaborate tetrahydrate |
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