CN1222485A - Preparation of light magnesium carbonate by using baron slurry - Google Patents

Preparation of light magnesium carbonate by using baron slurry Download PDF

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Publication number
CN1222485A
CN1222485A CN 97120985 CN97120985A CN1222485A CN 1222485 A CN1222485 A CN 1222485A CN 97120985 CN97120985 CN 97120985 CN 97120985 A CN97120985 A CN 97120985A CN 1222485 A CN1222485 A CN 1222485A
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container
pressure
magnesium carbonate
boric sludge
water
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CN 97120985
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CN1059876C (en
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李治涛
王秀峰
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Abstract

The preparation process consists of the steps of roast, digestion and carbonization successively. Compared with the prior art, the present preparation process has less filter residue, being only 30-70% of the amount of boron mud, and the filter residue is stable chemically and less prone to decompose and may be used in producing brick to utilize fully and eliminate environmental pollution.

Description

Method for preparing light magnesium carbonate by using boron mud
The invention relates to a method for preparing light carbonic acid, in particular to a method for preparing light magnesium carbonate by using boric sludge.
The light magnesium carbonate has wide application, is mainly used as a filling agent and a reinforcing agent of rubber products and a high-grade fireproof heat-insulating material, and can also be used in the manufacturing fields of various products such as food, medicine, pottery, paint, cosmetics, toothpaste and the like. The method for preparing light magnesium carbonate from boric sludge is known to date as a 'boric sludge causticization method', and the main defects of the method for preparing light magnesium carbonate are as follows: the waste residue formed after preparing the light magnesium carbonate is increased, usually 120 percent of the boron mud, and the main components of the waste residue are calcium carbonate, magnesium carbonate and the like,the waste residue is difficult to recycle, so that the resource utilization rate is reduced, and the environment is seriously polluted after the waste residue is abandoned.
The invention aims to provide a novel method for extracting light magnesium carbonate from boric sludge so as to recycle waste residue formed after extracting magnesium carbonate.
The object of the invention is achieved by the following process steps.
A. Roasting
Heating the boron mud to 850 ℃ at 550 ℃, roasting the boron mud at the temperature for not less than 2 hours, and naturally cooling the boron mud to room temperature;
B. digestion of
Putting a certain amount of roasted boric sludge into a container, measuring the total weight of magnesium oxide contained in the boric sludge, adding water into the boric sludge according to the weight part ratio of the magnesium oxide to the water of 1: 60-100, then heating the mixture of the boric sludge and the water to 90-95 ℃, digesting (preserving heat) for 10-60 minutes, and then cooling the mixture to be not more than 30 ℃;
C. carbonizing
Adding a certain amount of catalyst into the mixture of boric sludge and water in a container according to the determined weight of magnesium oxide and the ratio of the weight part of magnesium oxide to the weight part of catalyst of 100: 0.5-1, wherein the catalyst can be hydrochloric acid or nitric acid or ammonium salt or magnesium salt formed by the two acids, uniformly stirring, sealing the container, introducing pressurized kiln gas into the container to carbonize the container, and when the pressure of the kiln gas in the container reaches 2kg/cm2Then, maintaining the pressure for at least 1 hour; then, the pressureof kiln gas in the container is increased to 3kg/cm2Maintaining the pressure for a period of time until the liquid material is determined to be pink by phenolphthalein, and terminating the carbonization process; during the carbonization step, maintaining the temperature of the mixture in the vessel at not more than 30 ℃;
D. finished product
And C, filtering the slurry produced in the step C, removing filter residues, taking filtrate, heating the filtrate in a container to 85-97 ℃, and preserving heat for at least 10 minutes to pyrolyze the filtrate to generate light magnesium carbonate. Then, filtering out water, and drying a filter cake to obtain a light magnesium carbonate finished product.
The chemistry in each process step for preparing light magnesium carbonate from boric sludge is more as follows:
A. roasting
B. Digestion of
C. Carbonizing
(1)
(2)
Reducing the catalyst and then entering the process (1)
D. The obtained product has 85-95 deg.C
The method is used for preparing light magnesium carbonate from the boron mud, the filter residue amount is small and is only 30-70% of the cooked boron mud, and the main components of the filter residue are magnesium silicate, silicon dioxide, ferric oxide and the like which are not easy to decompose; therefore, compared with the prior art, the invention has the advantages of high utilization rate of boron mud resources, capability of eliminating the pollution to the environment and the like.
The present invention will be described in further detail with reference to examples.
Example one
1kg of boric sludge was charged into a high temperature furnace, heated to 700 ℃ and calcined at this temperature for 2 hours, and then cooled to room temperature.
Taking a proper amount of boron mud after roasting, and measuring the content of magnesium oxide to be 70%.
150g of boron mud after roasting is placed in a container. And the total weight of magnesium oxide in the 150g of boron sludge was calculated to be 105g, and accordingly, 6.3 liters of hot water at 90-95 ℃ was added to the vessel, digested (stacked temperature) for 10 minutes, and then cooled to 30 ℃.
Adding 1g ammonia chloride into the container, sealing the container, and introducing industrial kiln gas with carbon dioxide content of 28-33%The pressure of kiln gas in the container is made to be equal to 2kg/cm2. Keeping the pressure for 1 hour; then, the pressure of kiln gas in the container is increased to 3kg/cm2Maintaining the pressure for a period of time until the feed liquid is free of pink color as determined by phenolphthalein, and terminating the carbonization process; during this carbonization process, the vessel was cooled with water and the dissolution was more exothermic, keeping the vessel at 30 ℃.
Filtering the slurry in the container, removing filter residues, taking filtrate, heating the filtrate in a container to90 ℃, preserving heat for 10 minutes to pyrolyze the filtrate to generate magnesium carbonate, aging the magnesium carbonate for 10 minutes, filtering out water (namely, filter pressing), and drying a filter cake to obtain 112g of light magnesium carbonate product.
Example two
1kg of boric sludge was charged into a high temperature furnace, heated to 550 ℃ and calcined at this temperature for 2 hours and 30 minutes, and then cooled to room temperature.
Taking a proper amount of boron mud after roasting, and measuring the content of magnesium oxide to be 62%.
150g of boron sludge after calcination was placed in a vessel, and the total weight of magnesium oxide contained in the 150g of boron sludge was calculated to be 93g, whereby 6 liters of hot water at 90 to 95 ℃ was introduced into the vessel, digested (heat-preserved) for 10 minutes, and then cooled to 30 ℃.
Adding 1g of ammonia chloride into the container, sealing the container, introducing industrial kiln gas with carbon dioxide content of 28-33%' to make the pressure of kiln gas in the container equal to 2kg/cm2Keeping the pressure for 1 hour; then, the pressure of kiln gas in the container is increased to 3kg/cm2Maintaining the pressure for a period of time until the feed liquid is free of pink color as determined by phenolphthalein, and terminating the carbonization process; during this carbonization, the vessel was cooled with water, the disintegration should be more exothermic, and the temperature of the vessel was maintained at 30 ℃.
Filtering the slurry in the container, removing filter residues, taking filtrate, heating the filtrate in the container to 95 ℃, preserving heat for 10 minutes to pyrolyze the filtrate to generate magnesium carbonate, aging the magnesium carbonate for 10 minutes, filtering out water (namely, press-filtering), and drying a filter cake to obtain a light magnesium carbonate product 105 g.
EXAMPLE III
1kg of boric sludge was charged into a high temperature furnace, heated to 850 ℃ and calcined at this temperature for 1 hour 40 minutes, and then cooled to room temperature.
Taking a proper amount of boron mud after roasting, and measuring the content of magnesium oxide to be 60%.
150g of boron mud after roasting is placed in a container, the total weight of the fresh boron mud containing oxygen in 150g is calculated to be 90g, and according to the weight, 6 liters of hot water with the temperature of 90-95 ℃ is added into the container, and the mixture is digested (heat-preserved) for 10 minutes and then cooled to 30 ℃.
Adding 1g of ammonia chloride into the container, sealing the container, introducing industrial kiln gas with carbon dioxide content of 28-33%' to make the pressure of kiln gas in the container equal to 2kg/cm2Keeping the pressure for 1 hour; then, the pressure of kiln gas in the container is increased to 3kg/cm2Maintaining the pressure for a period of time until the feed liquid is free of pink color as determined by phenolphthalein, and terminating the carbonization process; during the carbonization process, the vessel was cooled with water, the exothermic decomposition reaction was released, and the temperature of the vessel was maintained at 30 ℃.
Filtering the slurry in the container, removing filter residues, taking filtrate, heating the filtrate to 97 ℃ in the container, preserving the heat for 10 minutes to pyrolyze the filtrate to generate magnesium carbonate, aging the magnesium carbonate for 10 minutes, filtering out water (namely, filter pressing), and drying a filter cake to obtain 101g of light magnesium carbonate product.

Claims (1)

1. The method for preparing light magnesium carbonate by using boric sludge is characterized by sequentially comprising the following process steps of:
A. roasting
Heating the boron mud to 850 ℃ at 550 ℃, roasting the boron mud at the temperature for not less than 2 hours, and naturally cooling the boron mud to room temperature;
B. digestion of
Putting a certain amount of roasted boric sludge into a container, measuring the total weight of magnesium oxide contained in the boric sludge, adding water into the boric sludge according to the weight part ratio of the magnesium oxide to the water of 1: 60-100, then heating the mixture of the boric sludge and the water to 90-95 ℃, digesting (preserving heat) for 10-60 minutes, and then cooling the mixture to be not more than 30 ℃;
c; carbonizing
Adding a certain amount of catalyst into the mixture of boric sludge and water in a container according to the determined weight of magnesium oxide and the ratio of the weight part of magnesium oxide to the weight part of catalyst of 100: 0.5-1, wherein the catalyst can be hydrochloric acid or nitric acid or ammonium salt or magnesium salt formed by the two acids, uniformly stirring, sealing the container, introducing pressurized kiln gas into the container to carbonize the container, and when the pressure of the kiln gas in the container reaches 2kg/cm2When the pressure is maintained, the pressure is maintained; maintaining the pressure for at least 1 hour; then, the pressure of kiln gas in the container is increased to 3kg/cm2Maintaining the pressure for a period of time until the liquid material is determined to be pink by phenolphthalein, and terminating the carbonization process; during the carbonization step, maintaining the temperature of the mixture in the vessel at not more than 30 ℃;
D. finished product
And C, filtering the slurry produced in the step C, removing filter residues, taking filtrate, heating the filtrate in a container to 85-97 ℃, preserving the heat for at least 10 minutes to pyrolyze the filtrate to generate light magnesium carbonate, then filtering water out, and drying filter cakes to obtain the light magnesium carbonate finished product.
CN97120985A 1997-12-05 1997-12-05 Preparation of light magnesium carbonate by using baron slurry Expired - Fee Related CN1059876C (en)

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Application Number Priority Date Filing Date Title
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CN1222485A true CN1222485A (en) 1999-07-14
CN1059876C CN1059876C (en) 2000-12-27

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1122636C (en) * 2001-03-19 2003-10-01 李洪岭 Process for recovering boric acid from boron mud
CN100558637C (en) * 2008-01-25 2009-11-11 吉林省新世纪农业科技有限公司 Produce the method for magnesium basic carbonate by boron mud
CN102424408A (en) * 2011-08-03 2012-04-25 深圳市信诺泰投资管理有限公司 Comprehensive utilization method of boric sludge
CN103923379A (en) * 2013-01-14 2014-07-16 中国地质大学(北京) Method for preparing fire retardation polymer composite material by using boron mud
CN103979584A (en) * 2014-06-03 2014-08-13 李广凡 Process for preparing light magnesium carbonate from boron mud
CN103979583A (en) * 2014-05-28 2014-08-13 李广凡 Method for preparing light magnesium carbonate by using boric sludge carbonization method
CN104418573A (en) * 2013-08-22 2015-03-18 丹东玉龙镁业有限公司 Method for comprehensive utilization of industrial waste boron sludge
CN108238617A (en) * 2018-03-22 2018-07-03 河北科技大学 A kind of method and anhydrous magnesium carbonate of carbonizatin method production anhydrous magnesium carbonate
CN109250735A (en) * 2017-07-13 2019-01-22 田利 A method of recycling trade waste boron mud

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1033081C (en) * 1993-09-13 1996-10-23 高佳令 Method for extracting light magnesium carbonate from boron mud

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1122636C (en) * 2001-03-19 2003-10-01 李洪岭 Process for recovering boric acid from boron mud
CN100558637C (en) * 2008-01-25 2009-11-11 吉林省新世纪农业科技有限公司 Produce the method for magnesium basic carbonate by boron mud
CN102424408A (en) * 2011-08-03 2012-04-25 深圳市信诺泰投资管理有限公司 Comprehensive utilization method of boric sludge
CN102424408B (en) * 2011-08-03 2013-11-13 深圳市信诺泰投资管理有限公司 Comprehensive utilization method of boric sludge
CN103923379A (en) * 2013-01-14 2014-07-16 中国地质大学(北京) Method for preparing fire retardation polymer composite material by using boron mud
CN103923379B (en) * 2013-01-14 2016-08-10 中国地质大学(北京) A kind of utilize boric sludge for the method for flame-retardant high-molecular composite
CN104418573A (en) * 2013-08-22 2015-03-18 丹东玉龙镁业有限公司 Method for comprehensive utilization of industrial waste boron sludge
CN103979583A (en) * 2014-05-28 2014-08-13 李广凡 Method for preparing light magnesium carbonate by using boric sludge carbonization method
CN103979584A (en) * 2014-06-03 2014-08-13 李广凡 Process for preparing light magnesium carbonate from boron mud
CN109250735A (en) * 2017-07-13 2019-01-22 田利 A method of recycling trade waste boron mud
CN108238617A (en) * 2018-03-22 2018-07-03 河北科技大学 A kind of method and anhydrous magnesium carbonate of carbonizatin method production anhydrous magnesium carbonate

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