CN109607550B - Deacidifying method for acid-washed quartz sand - Google Patents

Deacidifying method for acid-washed quartz sand Download PDF

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CN109607550B
CN109607550B CN201910012182.7A CN201910012182A CN109607550B CN 109607550 B CN109607550 B CN 109607550B CN 201910012182 A CN201910012182 A CN 201910012182A CN 109607550 B CN109607550 B CN 109607550B
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quartz sand
acid
alkaline
parts
clay
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CN109607550A (en
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赵祥
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Linyi Haoquan Silicon Technology Co ltd
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    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12Naturally occurring clays or bleaching earth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
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Abstract

The invention discloses a deacidification method for acid-washed quartz sand, and belongs to the technical field of quartz sand preparation. The adsorption balls with strong adsorption function are added in the acid washing process link of the quartz sand, so that the purity of the quartz sand is improved, the rapid removal of acid liquor is facilitated, and the acid washing method has the advantages of simple process and good acid washing effect.

Description

Deacidifying method for acid-washed quartz sand
Technical Field
The invention belongs to the technical field of quartz sand production, and particularly relates to a deacidification method for acid-washed quartz sand.
Background
The quartz sand has the advantages of good heat resistance, corrosion resistance, rich resources, low price and the like, and is widely applied. The quartz sand is one of the most common non-metallic mineral raw materials in the nature, and along with the rapid development of national economy and science and technology, the application of the quartz sand is not limited to the traditional fields of glass products, building materials and the like which have low requirements on the quality of raw materials any more, and the quartz sand starts to be involved in the high and new technology industry field, and has low or even no requirements on the quality of common glass and building sand; for the sand used for fine and high-performance materials such as electronic materials, quartz crucibles and the like, the requirements on the quality of raw materials are strict, high-purity and ultra-pure quartz sand is needed, and the requirement on the total content of impurities is very low. In the purification of quartz sand, acid pickling is one of the methods commonly used by people, and acid liquor of the pickled quartz sand often remains on the surface of the quartz sand and can influence the subsequent processing procedures, so that the acid pickling treatment of the pickled quartz sand is required. The applicant found that the national patent office discloses a method and a device for continuous acid washing and purifying quartz sand with patent number 201410341084.5, wherein (4) deacidification: removing acid liquor in the quartz sand discharged from the pickling container by using a dewatering screen or a centrifugal machine; (5) washing with water: conveying the deacidified quartz sand to washing equipment, and washing until the pH value is neutral; and a patent with patent number 201610527263.7 for a large-scale quartz sand pickling, impurity removing and whitening process, wherein the quartz sand after the reaction in the step (4) enters a sand washing device for circularly adding water for cleaning and deacidifying; (5) and (4) draining the deacidified quartz sand in a finished product warehouse to obtain the finished product quartz sand. In the processes, water is used for washing, and for the quartz sand which is soaked by a large amount of concentrated acid before, particularly washed by hydrochloric acid or nitric acid, the washing is not thorough enough, residual chloride ions or nitrate ions and the like remain on the surface of the washed quartz sand, so that the washed quartz sand is yellowed in color, the product value is influenced due to poor appearance, and the processing performance is also influenced.
Disclosure of Invention
In order to overcome the defects, the invention provides a deacidification method for acid-washed quartz sand.
The invention aims to realize the purpose through the following technical scheme, and the deacidification method for the acid-washed quartz sand comprises the following steps:
(1) feeding the quartz sand to be purified and pickled into a pickling reaction tank through a feeding machine;
(2) heating quartz sand to 80-120 ℃, adding a mixed solution of 30-40% sulfuric acid, 15-25% fluosilicic acid and 15-30% nitric acid, continuously stirring and mixing the acid solution and the quartz sand for 20min, standing for 3-5h, continuously stirring for 20min, standing for 1-2h, discharging the acid solution remained in an acid washing reaction tank, and recovering the acid solution into an acid solution recovery storage tank;
(3) and (2) feeding the scrubbed quartz sand into a sand washing device, washing and deacidifying the scrubbed quartz sand once, then discharging water, adding clean water which is 20-30cm over the quartz sand, adding an adsorption ball, stirring for 15-30min, standing for 30min, stirring for 10-20min at an accelerated speed, standing for 30min, continuously adding water for washing, separating the adsorption ball due to the large volume of the adsorption ball by a filtering method, circularly adding water for washing for 2-3 times over the separated quartz sand, and then feeding the quartz sand into a finished product warehouse for draining.
Preferably, the adding amount of the adsorption balls is 0.8-1.2% of the weight of the quartz sand.
The adsorption ball is prepared from 9-16 parts of alkaline clay, 3-12 parts of chitosan, 30-45 parts of alkaline ash and 10-20 parts of turpentine oil.
The preferred adsorption ball is prepared from 12 parts of alkaline clay, 7 parts of chitosan, 38 parts of alkaline ash and 15 parts of turpentine oil.
The preparation method of the alkaline clay comprises the following steps: weighing 50kg of activated clay into a container, adding 45L of water, uniformly stirring, and weighing calcium oxide accounting for 80% of the mass fraction of the activated clay to prepare emulsion for later use; adding the calcium oxide emulsion into activated clay, reacting at 70 deg.C for 6-10h, vacuum filtering, oven drying at 50-60 deg.C, and grinding to 80-100 mesh to obtain alkaline clay.
The alkaline ash is prepared by mixing and crushing corn straws and castor straws according to the weight ratio of 5:1, calcining for 10-12h at the temperature of 700-800 ℃, and crushing for 60-80 meshes.
The preparation method of the adsorption ball comprises the following steps: uniformly mixing the selected alkaline clay, chitosan and alkaline ash in parts by weight, adding turpentine oil to prepare a soft material, extruding the soft material through a sieve with a proper pore diameter by using the pressure of an extruder, after forming a round-like cylindrical strip shape, putting the round-like cylindrical strip shape into a rapidly rotating rounding machine to prepare a pill with the diameter of 3-6cm, and standing and drying for 48-72 hours at normal temperature to obtain the finished product.
The applicant researches and discovers that in the process of stirring the adsorption balls and the quartz sand, the quartz sand continuously impacts the adsorption balls from all directions, the quartz sand is continuously rebounded due to the fact that the adsorption balls are high in mass, and in the process, cracks occur again in some quartz sand particles, so that further acid washing and adsorption of the adsorption balls on impurities are facilitated; even if no crack is generated after the quartz sand particles and the adsorption balls are impacted, the quartz sand is vibrated when the quartz sand particles and the adsorption balls are contacted, so that the adsorption balls can adsorb impurities; when the surface of the adsorption ball neutralizes part of the acid liquid, a rough surface is formed, which is more beneficial to the adsorption of impurities.
The invention has the beneficial effects that: at present, no report or record about the combination of alkaline clay, chitosan, alkaline ash and turpentine oil exists, and no report or record about the application of the alkaline clay, the chitosan, the alkaline ash and the turpentine oil to the deacidification and purification of quartz sand after being prepared into an adsorbent is found; in the deacidification process of quartz sand, the adsorption balls are added, so that the deacidification effect is thorough, and the SiO is obviously improved2The content and the impurity removal effect are obvious, and the application range of the quartz sand is widened; the method is simple, practical and easy to operate.
The quartz sand prepared according to the quartz sand preparation step of the invention is set as group A, and the quartz sand prepared without adding an adsorption ball is set as group B according to a conventional method; the specific experimental data for each group are shown in the table below.
Group of SiO2Content (%) Fe2O3Content (%) A1203Content (%) T i0 2Content (percent)) Acidity
Group B 98.7542 0.102 0.142 0.019 Weak acidity
Group A 99.9410 0.031 0.017 0.0011 Neutral property
According to the data, the deacidification effect is obvious after the adsorption balls are added, and SiO in the group A is obtained2The content reaches 99.9410%, and the ideal effect is achieved.
Detailed Description
The first embodiment is as follows: a deacidification method for acid-washed quartz sand comprises the following steps: (1) feeding the quartz sand to be purified and pickled into a pickling reaction tank through a feeding machine; (2) heating quartz sand to 90 ℃, adding a mixed solution of 35% sulfuric acid, 20% fluosilicic acid and 20% nitric acid, continuously stirring and mixing the acid solution and the quartz sand for 20min, standing for 4h, continuously stirring for 20min, standing for 2h, discharging the acid solution remained in an acid washing reaction tank, and recovering the acid solution into an acid solution recovery storage tank; (3) and (2) feeding the scrubbed quartz sand into a sand washing device, washing and deacidifying the scrubbed quartz sand once, then discharging water, then adding clear water which is 25cm over the quartz sand, adding an adsorption ball, stirring for 20min, standing for 30min, stirring again for 15min, standing for 30min, continuously adding water for washing, separating the adsorption ball by a filtering method due to large volume of the adsorption ball, circularly adding water for washing for 2 times, and then feeding the separated quartz sand into a finished product warehouse for draining. Preferably, the amount of the adsorption balls added is 1% of the weight of the quartz sand in the equipment. The adsorption ball is prepared from 12 parts of alkaline clay, 7 parts of chitosan, 38 parts of alkaline ash and 15 parts of turpentine oil. The preparation method of the alkaline clay comprises the following steps: weighing 50kg of activated clay into a container, adding 45L of water, uniformly stirring, and weighing calcium oxide accounting for 80% of the mass fraction of the activated clay to prepare emulsion for later use; adding the calcium oxide emulsion into activated clay in batches, carrying out heat preservation reaction at 70 ℃ for 8 hours, carrying out suction filtration, drying at 55 ℃, and grinding through a 90-mesh sieve to obtain the alkaline clay. The alkaline ash is prepared by mixing and crushing corn straws and castor straws according to the weight ratio of 5:1, calcining for 11 hours at 750 ℃ and crushing to 70 meshes. The preparation method of the adsorption ball comprises the following steps: uniformly mixing the selected alkaline clay, chitosan and alkaline ash in parts by weight, adding turpentine oil to prepare a soft material, extruding the soft material through a sieve with a proper pore diameter by using the pressure of an extruder, after forming a round-like cylindrical strip shape, putting the round-like cylindrical strip shape into a rapidly rotating rounding machine to prepare a pill with the diameter of 4cm, and standing and drying the pill at normal temperature for 60 hours to obtain the finished product.
Example two: a deacidification method for acid-washed quartz sand comprises the following steps: (1) feeding the quartz sand to be purified and pickled into a pickling reaction tank through a feeding machine; (2) heating quartz sand to 80 ℃, adding a mixed solution of 30% sulfuric acid, 15% fluosilicic acid and 15% nitric acid, continuously stirring and mixing the acid solution and the quartz sand for 20min, standing for 3h, continuously stirring for 20min, standing for 1h, discharging the acid solution remained in an acid washing reaction tank, and recovering the acid solution into an acid solution recovery storage tank; (3) and (2) feeding the scrubbed quartz sand into a sand washing device, washing and deacidifying the scrubbed quartz sand once, then discharging water, adding clean water which is 20cm over the quartz sand, adding an adsorption ball, stirring for 15min, standing for 30min, stirring for 10min again, standing for 30min, continuously adding water for washing, separating the adsorption ball by a filtering method because the adsorption ball is large in size, circularly adding water for washing for 2 times, and then feeding the separated quartz sand into a finished product warehouse for draining. Preferably, the amount of the adsorption balls added is 0.8% of the weight of the quartz sand in the equipment. The adsorption ball is prepared from 9 parts of alkaline clay, 3 parts of chitosan, 30 parts of alkaline ash and 10 parts of turpentine oil. The preparation method of the alkaline clay comprises the following steps: weighing 50kg of activated clay into a container, adding 45L of water, uniformly stirring, and weighing calcium oxide accounting for 80% of the mass fraction of the activated clay to prepare emulsion for later use; adding the calcium oxide emulsion into activated clay in batches, carrying out heat preservation reaction at 70 ℃ for 6 hours, carrying out suction filtration, drying in an environment at 50 ℃, and grinding through a 80-mesh sieve to obtain the alkaline clay. The alkaline ash is prepared by mixing and crushing corn straws and castor straws according to the weight ratio of 5:1, calcining for 10 hours at 700 ℃, and crushing for 60 meshes. The preparation method of the adsorption ball comprises the following steps: uniformly mixing the selected alkaline clay, chitosan and alkaline ash in parts by weight, adding turpentine oil to prepare a soft material, extruding the soft material through a sieve with a proper pore diameter by using the pressure of an extruder, after forming a round-like cylindrical strip shape, putting the round-like cylindrical strip shape into a rapidly rotating rounding machine to prepare a pill with the diameter of 3cm, and standing and drying for 48 hours at normal temperature to obtain the finished product.
Example three: a deacidification method for acid-washed quartz sand comprises the following steps: (1) feeding the quartz sand to be purified and pickled into a pickling reaction tank through a feeding machine; (2) heating quartz sand to 120 ℃, adding a mixed solution of 40% sulfuric acid, 25% fluosilicic acid and 30% nitric acid, continuously stirring and mixing the acid solution and the quartz sand for 20min, standing for 5h, continuously stirring for 20min, standing for 2h, discharging the acid solution remained in an acid washing reaction tank, and recovering the acid solution into an acid solution recovery storage tank; (3) and (2) feeding the scrubbed quartz sand into a sand washing device, washing and deacidifying the scrubbed quartz sand once, then discharging water, adding clear water which is 30cm over the quartz sand, adding an adsorption ball, stirring for 30min, standing for 30min, stirring for 20min again, standing for 30min, continuously adding water for washing, separating the adsorption ball by a filtering method because the adsorption ball is large in size, circularly adding water for washing for 3 times, and then feeding the separated quartz sand into a finished product warehouse for draining. Preferably, the amount of the adsorption balls added is 1.2% of the weight of the quartz sand in the equipment. The adsorption ball is prepared from 16 parts of alkaline clay, 12 parts of chitosan, 45 parts of alkaline ash and 20 parts of turpentine oil. The preparation method of the alkaline clay comprises the following steps: weighing 50kg of activated clay into a container, adding 45L of water, uniformly stirring, and weighing calcium oxide accounting for 80% of the mass fraction of the activated clay to prepare emulsion for later use; adding the calcium oxide emulsion into activated clay in batches, carrying out heat preservation reaction at 70 ℃ for 10 hours, carrying out suction filtration, drying at 60 ℃, and grinding through a 100-mesh sieve to obtain the alkaline clay. The alkaline ash is prepared by mixing and crushing corn straws and castor straws according to the weight ratio of 5:1, calcining for 12 hours at 800 ℃, and crushing into 80 meshes. The preparation method of the adsorption ball comprises the following steps: uniformly mixing the selected alkaline clay, chitosan and alkaline ash in parts by weight, adding turpentine oil to prepare a soft material, extruding the soft material through a sieve with a proper pore diameter by using the pressure of an extruder, after forming a round-like cylindrical strip shape, putting the round-like cylindrical strip shape into a rapidly rotating rounding machine to prepare pills with the diameter of 6cm, and standing and drying for 72 hours at normal temperature to obtain the finished product.

Claims (3)

1. A deacidification method for acid-washed quartz sand is characterized by comprising the following steps: feeding the quartz sand to be purified and pickled into a pickling reaction tank through a feeding machine; heating quartz sand to 80-120 ℃, adding a mixed solution of 30-40% sulfuric acid, 15-25% fluosilicic acid and 15-30% nitric acid, continuously stirring and mixing the acid solution and the quartz sand for 20min, standing for 3-5h, continuously stirring for 20min, standing for 1-2h, discharging the acid solution remained in an acid washing reaction tank, and recovering the acid solution into an acid solution recovery storage tank; the washed quartz sand enters a sand washing device, is added with water, is washed and deacidified once, is drained, is added with clear water which is 20-30cm submerged in the quartz sand, is added with an adsorption ball, is stirred for 15-30min and then is kept stand for 30min, is stirred for 10-20min again and then is kept stand for 30min, is continuously added with water for washing, is separated out by a filtering method due to the large volume of the adsorption ball, and is circularly added with water for washing for 2-3 times and then enters a finished product warehouse for draining; the adsorption ball is prepared from 9-16 parts of alkaline clay, 3-12 parts of chitosan, 30-45 parts of alkaline ash and 10-20 parts of turpentine oil; the preparation method of the alkaline clay comprises the following steps: weighing 50kg of activated clay into a container, adding 45L of water, uniformly stirring, and weighing calcium oxide accounting for 80% of the mass fraction of the activated clay to prepare emulsion for later use; adding the calcium oxide emulsion into activated clay, keeping the temperature at 70 ℃ for reaction for 6-10h, performing suction filtration, drying at 50-60 ℃, and grinding through 80-100 meshes to obtain alkaline clay; the alkaline ash is prepared by mixing and crushing corn straws and castor straws according to the weight ratio of 5:1, calcining for 10-12h at the temperature of 700-800 ℃, and crushing for 60-80 meshes.
2. The method for deacidifying pickled quartz sand according to claim 1, wherein said method for preparing adsorption balls comprises the following steps: uniformly mixing the selected alkaline clay, chitosan and alkaline ash in parts by weight, adding turpentine oil to prepare a soft material, extruding the soft material through a sieve with a proper pore diameter by using the pressure of an extruder, after forming a round-like cylindrical strip shape, putting the round-like cylindrical strip shape into a rapidly rotating rounding machine to prepare a pill with the diameter of 3-6cm, and standing and drying for 48-72 hours at normal temperature to obtain the finished product.
3. The deacidification method for acid-washed quartz sand according to claim 1, wherein the addition amount of the adsorption balls is 0.8-1.2% by weight of the quartz sand.
CN201910012182.7A 2019-01-07 2019-01-07 Deacidifying method for acid-washed quartz sand Active CN109607550B (en)

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CN113321216B (en) * 2021-06-22 2023-09-22 中国地质科学院郑州矿产综合利用研究所 Method for preparing high-purity quartz by using quartz vein type tungsten waste stone

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Publication number Priority date Publication date Assignee Title
CN105948060A (en) * 2016-04-28 2016-09-21 江苏泽龙石英有限公司 Depickling method for pickled quartz sands
CN106185953A (en) * 2016-07-06 2016-12-07 王林 A kind of large-scale quartz sand pickling impurity removal whitening process

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CN101658783A (en) * 2009-09-15 2010-03-03 广西大学 Loaded calcium hydroxide activity carclazyte and preparation method thereof
CN105692629B (en) * 2016-04-28 2017-12-08 江苏泽龙石英有限公司 The method that acid-washed quartz sand is quickly cleaned
CN108455618B (en) * 2018-01-19 2021-08-06 徐州市万达石英有限公司 Process for large-scale circular pickling of quartz sand

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105948060A (en) * 2016-04-28 2016-09-21 江苏泽龙石英有限公司 Depickling method for pickled quartz sands
CN106185953A (en) * 2016-07-06 2016-12-07 王林 A kind of large-scale quartz sand pickling impurity removal whitening process

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