CN104944817A - Recycling method of sulfate process titanium dioxide by-product titanium gypsum - Google Patents

Recycling method of sulfate process titanium dioxide by-product titanium gypsum Download PDF

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Publication number
CN104944817A
CN104944817A CN201510296845.4A CN201510296845A CN104944817A CN 104944817 A CN104944817 A CN 104944817A CN 201510296845 A CN201510296845 A CN 201510296845A CN 104944817 A CN104944817 A CN 104944817A
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titanium
gypsum
composite
powder
titanium gypsum
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CN201510296845.4A
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李亮
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Panzhihua University
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Panzhihua University
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Abstract

The invention discloses a recycling method of a sulfate process titanium dioxide by-product titanium gypsum and a wall material prepared from the titanium gypsum. The invention belongs to the field of resource recycling. The method comprises steps of dehydration treatment, calcining treatment, fine grinding treatment, compounding treatment, mixing treatment, natural curing and roasting treatment which are carried out on the titanium gypsum. By the method, titanium gypsum is reasonably utilized by modified compounding treatment of titanium gypsum, and the prepared gypsum block wall material meets requirements of performance index, has characteristics of environmental protection and low cost and is suitable for popularization and application.

Description

Sulfate process titanium dioxide by-product titanium gypsum regeneration method and the materials for wall made
Technical field
The invention belongs to resource recycling field, the materials for wall being specifically related to a kind of sulfate process titanium dioxide by-product titanium gypsum regeneration method and making.
Background technology
Panzhihua Region has very abundant v-ti magnetite ore resources, vanadium titano-magnetite can select vanadium iron concentrate and ilmenite concentrate through ore dressing, ilmenite concentrate can be directly used in Titanium White Production By Sulfuric Acid Process, also titanium slag can be produced through smelting, titanium slag can be used for Production By Sulfuric Acid Process titanium white, the advantage of Production By Sulfuric Acid Process titanium white is less investment, constant product quality, weak point is that three wastes discharge amount is larger, the three wastes mainly contain waste gas, waste residue and waste water, wherein waste water mainly acid waste water, for the process of acid waste water, the general processing mode of each industry is all adopt the mode of limestone vegetation to discharge, middle ash has the low advantage of processing cost, weak point to bring secondary pollution, adopt Production By Sulfuric Acid Process titanium white according to statistics, often produce the titanium gypsum that one ton of titanium white will produce about 4 ~ 4.5 tons, the titanium gypsum produced is piled up gradually, land occupation resource on the one hand, on the one hand more serious pollution is caused to environment.Titanium gypsum complex chemical composition, foreign matter content is higher, there is larger difference with the performance of the plaster of paris, and the Application and Development of titanium gypsum exists larger technical difficulty.Only have and titanium gypsum just can be made to be developed and applied by special technical finesse.Panzhihua City government makes in the process of " vanadium titanium all " with all strength in recent years, many sulfate process titanium dioxide factories have progressively been built in Panzhihua Region, the generation of titanium gypsum is anxious to be increased, the comprehensive utilizating research work carrying out titanium gypsum not yet in effect in recent years, titanium gypsum land occupation resource and show outstanding especially to the pollution problem that environment brings, in this case, how research disposes the work that titanium gypsum has become the most important thing.Reasonable disposal titanium gypsum is also fully utilized, and the safely cleaning that will promote Panzhihua Region sulfate process titanium dioxide is further produced, and significant to developing of Panzhihua Region titanium industry.
Summary of the invention
The materials for wall that technical problem to be solved by this invention is to provide a kind of sulfate process titanium dioxide by-product titanium gypsum regeneration method and makes.
The technical solution adopted for the present invention to solve the technical problems is: sulfate process titanium dioxide by-product titanium gypsum regeneration method, comprises the steps:
A, first employing filter plant carry out processed to titanium gypsum;
B, to dehydration after titanium gypsum carry out calcination processing;
C, to calcining after titanium gypsum carry out levigate process;
D, carry out complex treatment to the titanium gypsum after levigate, composite material comprises properties-correcting agent and retardant; The composite amount of titanium gypsum is 50 ~ 85 weight parts;
Described properties-correcting agent is one or more in calcining natural gesso, calcining desulfurization gypsum powder, magnesia powder and silicon powder composite powder, Portland clinker; When composite Material selec-tion calcining natural gesso or desulfurization gypsum powder, the composite amount of calcining natural gesso or desulfurization gypsum powder is 30 ~ 60 weight parts; When composite Material selec-tion Portland clinker, the composite amount of Portland clinker is 10 ~ 25 weight parts; When composite Material selec-tion magnesia powder and silicon powder composite powder, the composite amount of magnesia powder and silicon powder composite powder is 5 ~ 15 weight parts;
Described retardant is one or more in sodium polyphosphate, borax, citric acid, sodium-metaphosphate; The composite amount of retardant is 0.02 ~ 4 weight part;
E, combination treatment is carried out to the raw material after composite, after mixing, then add after a certain proportion of water mixes, adopt that casting is shaping makes titanium gypsum blockwork material;
F, natural curing process is carried out to the titanium gypsum blockwork material made;
Carry out baking processing after g, natural curing process, obtain titanium gypsum blockwork finished material.
Wherein, described calcining natural gesso, calcining desulfurization gypsum powder, magnesia powder and silicon powder composite powder, Portland clinker market are all on sale, calcining natural gesso or calcining desulfurization gypsum powder refer to natural gesso through calcination processing or desulfurization gypsum powder, calcining temperature is usually at 170 ~ 220 DEG C, and calcination time is usually at 1 ~ 3 hour.The preferred borax of described retardant.
Wherein, in aforesaid method, the composite material of steps d also comprises vegetable fibre and/or paper fiber, and the composite amount of vegetable fibre and paper fiber is 1 ~ 6 weight part.Preferred employing vegetable fibre is allocated into separately.
Further, the length of vegetable fibre and paper fiber is preferably 1 ~ 3mm.Paper fiber preferably adopts waste paper fragmentation obtained.
Wherein, after adopting filter plant to carry out processed to titanium gypsum in aforesaid method step a, the water content of titanium gypsum is less than 10%.
Wherein, when calcining in aforesaid method step b, calcining top temperature controls at 170 ~ 220 DEG C, and this temperature lower calcination time controling was at 1 ~ 3 hour.
Wherein, require during levigate process in aforesaid method step c that granularity is greater than 200 orders.
Wherein, in aforesaid method steps d, the granularity of described calcining natural gesso, calcining desulfurization gypsum powder, magnesia powder and silicon powder composite powder, Portland clinker is all greater than 200 orders.
Wherein, in aforesaid method step e, the add-on of water is 80 ~ 110% of composite rear raw material gross weight.
Wherein, in aforesaid method step g, storing temperature controls at 80 ~ 120 DEG C, and baking time controlled at 12 ~ 36 hours.
The present invention also provides titanium gypsum blockwork material, is namely to be obtained by any one method above-mentioned.
The invention has the beneficial effects as follows: the present invention adopts titanium gypsum as main raw material that there is environmental protection, feature with low cost; The present invention is by calcining, levigate, composite, mixing, maintenance, baking processing, particularly by adding one or more in the properties-correcting agent plaster of paris, desulfurated plaster, Portland clinker and magnesia powder and silicon powder composite powder, add in thread waste paper fibre and vegetable fibre one or both, add the measure of retardant, titanium gypsum can not only be made reasonably to be utilized, and obtained gypsum block wall material meets the requirement of its performance index, is worthy of popularization.
Embodiment
Sulfate process titanium dioxide by-product titanium gypsum regeneration method of the present invention, comprises the steps:
A, first employing filter plant carry out processed to titanium gypsum;
B, to dehydration after titanium gypsum carry out calcination processing;
C, to calcining after titanium gypsum carry out levigate process;
D, carry out complex treatment to the titanium gypsum after levigate, composite material comprises properties-correcting agent and retardant; The composite amount of titanium gypsum is 50 ~ 85 weight parts;
Described properties-correcting agent is one or more in calcining natural gesso, calcining desulfurization gypsum powder, magnesia powder and silicon powder composite powder, Portland clinker; When composite Material selec-tion calcining natural gesso or desulfurization gypsum powder, the composite amount of calcining natural gesso or desulfurization gypsum powder is 30 ~ 60 weight parts; When composite Material selec-tion Portland clinker, the composite amount of Portland clinker is 10 ~ 25 weight parts; When composite Material selec-tion magnesia powder and silicon powder composite powder, the composite amount of magnesia powder and silicon powder composite powder is 5 ~ 15 weight parts;
Described retardant is one or more in sodium polyphosphate, borax, citric acid, sodium-metaphosphate; The composite amount of retardant is 0.02 ~ 4 weight part;
E, combination treatment is carried out to the raw material after composite, after mixing, then add after a certain proportion of water mixes, adopt that casting is shaping makes titanium gypsum blockwork material;
F, natural curing process is carried out to the titanium gypsum blockwork material made;
Carry out baking processing after g, natural curing process, obtain titanium gypsum blockwork finished material.
In the present invention, add the calcining plaster of paris and calcining desulfurated plaster, condensation and the aggregation extent of semi-hydrated gypsum colloidal particle in titanium gypsum can be strengthened, reduce impurity to the impact of the condensation of semi-hydrated gypsum in titanium gypsum, promote titanium gypsum condensation, play enhancement; Add fine magnesium oxide micro-powder and silicon powder composite powder, silicon powder can absorb the impurity component MgO in titanium gypsum, and form gel, MgO micro mist can absorb the SiO in titanium gypsum 2impurity forms gel, promotes the condensation of impurity component in titanium gypsum; Add Portland clinker, during Portland clinker aquation, can gel be produced, absorb free CaO impurity in titanium gypsum, effect is cured to impurity phase.Preferred calcining desulfurization gypsum powder is as built agent, and desulfurization gypsum powder is the by product of flue gas desulfurization, desulfurization gypsum powder can be recycled, and reduces environmental pollution, saves plaster of paris resource.
Preferably, in aforesaid method, the composite material of steps d also comprises vegetable fibre and/or paper fiber, and the composite amount of vegetable fibre and paper fiber is 1 ~ 6 weight part.Preferred employing vegetable fibre is allocated into separately.Further, the length of vegetable fibre and paper fiber is preferably 1 ~ 3mm.
Preferably, after adopting filter plant to carry out processed to titanium gypsum in aforesaid method step a, the water content of titanium gypsum is less than 10%.Processed of the present invention makes titanium gypsum water content more few better, can save the energy consumption of lower step calcination processing.Processed can adopt filter plant centrifugal filter, plate-and-frame filter press, prioritizing selection plate-and-frame filter press.
Preferably, when calcining in aforesaid method step b, calcining top temperature controls at 170 ~ 220 DEG C, and this temperature lower calcination time controling was at 1 ~ 3 hour.Can industrial exhaust heat be made full use of in calcination process, reduce calcining cost.Calciner can select shaft kiln, rotary kiln etc., prioritizing selection rotary kiln.
Preferably, require during levigate process in aforesaid method step c that granularity is greater than 200 orders.Levigate equipment can select Raymond mill, ball mill etc., prioritizing selection ball mill.
Preferably, in aforesaid method steps d, the granularity of described calcining natural gesso, calcining desulfurization gypsum powder, magnesia powder and silicon powder composite powder, Portland clinker is all greater than 200 orders.
Preferably, in aforesaid method step e, the add-on of water is 80 ~ 110% of composite rear raw material gross weight.The material mixed should in 10min casting complete, ancillary vibration equipment can be adopted in casting process, ensure shaping fully tight.Casting 0.5 ~ 2 day rear collapsible die, the titanium gypsum materials for wall work in-process after form removal can carry out baking processing through natural curing in 1 ~ 2 day.
Preferably, in aforesaid method step g, storing temperature controls at 80 ~ 120 DEG C, and baking time controlled at 12 ~ 36 hours.Roasting plant can select tunnel like roasting kiln, can make full use of industrial exhaust heat.
The present invention also provides titanium gypsum blockwork material, is namely to be obtained by any one method above-mentioned.
Below by embodiment, the specific embodiment of the invention is described further, but not therefore by protection scope of the present invention restriction in one embodiment.
The process that embodiment adopts is as follows:
1, dewater: select plate-and-frame filter press to carry out processed to sulfuric acid process by-product titanium gypsum, guarantee that titanium gypsum water content is lower than 10%.
2, calcine: select rotary kiln to carry out calcination processing to the titanium gypsum after dehydration, guarantee that dihydrate gypsum is all transformed into semi-hydrated gypsum, calcining temperature controls at 170 ~ 220 DEG C, and this temperature lower calcination period is 1 ~ 3 hour.
3, composite: accurately to take raw material of the present invention and carry out composite.
4, mix: adopt Forced Mixing equipment and mix, add the water of 100%, ensure that mixing is full and uniform.
5, shaping: adopt cast shaping process to carry out shaping, the dimensional requirement according to materials for wall carries out die design, and mould is for convenience detach to be reused.
6, maintenance baking: after the demoulding, natural curing carried out baking processing after 1 ~ 2 day, and storing temperature controls at 80 ~ 120 DEG C, and baking time controls at two days, roasting plant selects tunnel drying kiln.
Embodiment
The preparation of materials for wall is carried out, component design following (formula 1-5 is corresponding table 1-table 5 respectively) according to said process:
Table 1 does not add formula of modifier
Material name Fineness, mm Proportioning (weight part)
Calcining titanium gypsum powder <0.088 100
Citric acid <0.088 0.2 is additional
Table 2 adds calcining natural gesso modified formula
Material name Fineness, mm Proportioning (weight part)
Calcining titanium gypsum powder <0.088 60
Calcining natural gesso <0.088 40
Citric acid <0.088 0.2 is additional
Table 3 adds calcining desulfurization gypsum powder modified formula
Material name Fineness, mm Proportioning (weight part)
Calcining titanium gypsum powder <0.088 60
Calcining desulfurization gypsum powder <0.088 40
Citric acid <0.088 0.2 is additional
Table 4 adds Portland clinker modified formula
Material name Fineness, mm Proportioning (weight part)
Calcining titanium gypsum powder <0.088 85
Portland clinker <0.088 15
Citric acid <0.088 0.2 is additional
Table 5 adds fiber prescription
Material name Fineness, mm Proportioning (weight part)
Calcining titanium gypsum powder <0.088 81
Portland clinker <0.088 15
Vegetable fibre Length 1-3mm 4
Citric acid <0.088 0.2 is additional
Size 240mm × 114mm × the 65mm of casting, form removal after shaping 1 day, after form removal after natural curing in 1 day, enter tunnel like roasting kiln baking processing, finally detect finished product, result is as follows:
1 average strength of filling a prescription is 2MPa, and 2 average strengths of filling a prescription are 4.7MPa, 3 average strengths of filling a prescription are 4.3MPa, formula semi-finals degree mean value is 4.9MPa, 5 average strengths of filling a prescription are 5.5MPa.
As can be seen from above detected result, directly adopt calcining titanium gypsum powder to produce gypsum block wall material and can not meet national standard requirement, properties-correcting agent of the present invention is absolutely necessary, and can have a strong impact on final product quality of the present invention.After composite by modification, intensity is improved, and can meet national standard requirement.
This shows, the inventive method can obtain superior in quality materials for wall.
As can be seen from formula 2 and formula 3, replace natural calcined gypsum powder as properties-correcting agent with desulfurization calcined gypsum powder, intensity is more or less the same, and as can be seen here, desulfurated plaster and the plaster of paris can become the good properties-correcting agent of the present invention, obtained superior in quality materials for wall.
From formula 4, add Portland clinker, also can improve the intensity of materials for wall, Portland clinker also can as properties-correcting agent.
Combined formulation 4 is known with formula 5, adds the intensity that vegetable fibre can improve materials for wall further, can strengthen the heat insulation effect of materials for wall simultaneously.

Claims (10)

1. sulfate process titanium dioxide by-product titanium gypsum regeneration method, is characterized in that comprising the steps:
A, first employing filter plant carry out processed to titanium gypsum;
B, to dehydration after titanium gypsum carry out calcination processing;
C, to calcining after titanium gypsum carry out levigate process;
D, carry out complex treatment to the titanium gypsum after levigate, composite material comprises properties-correcting agent and retardant; The composite amount of titanium gypsum is 50 ~ 85 weight parts;
Described properties-correcting agent is one or more in calcining natural gesso, calcining desulfurization gypsum powder, magnesia powder and silicon powder composite powder, Portland clinker; When composite Material selec-tion calcining natural gesso or desulfurization gypsum powder, the composite amount of calcining natural gesso or desulfurization gypsum powder is 30 ~ 60 weight parts; When composite Material selec-tion Portland clinker, the composite amount of Portland clinker is 10 ~ 25 weight parts; When composite Material selec-tion magnesia powder and silicon powder composite powder, the composite amount of magnesia powder and silicon powder composite powder is 5 ~ 15 weight parts;
Described retardant is one or more in sodium polyphosphate, borax, citric acid, sodium-metaphosphate; The composite amount of retardant is 0.02 ~ 4 weight part;
E, combination treatment is carried out to the raw material after composite, after mixing, then add after a certain proportion of water mixes, adopt that casting is shaping makes titanium gypsum blockwork material;
F, natural curing process is carried out to the titanium gypsum blockwork material made;
Carry out baking processing after g, natural curing process, obtain titanium gypsum blockwork finished material.
2. sulfate process titanium dioxide by-product titanium gypsum regeneration method according to claim 1, is characterized in that: the composite material of steps d also comprises vegetable fibre and/or paper fiber, and the composite amount of vegetable fibre and paper fiber is 1 ~ 6 weight part.
3. sulfate process titanium dioxide by-product titanium gypsum regeneration method according to claim 1 and 2, is characterized in that: after adopting filter plant to carry out processed to titanium gypsum in step a, the water content of titanium gypsum is less than 10%.
4. sulfate process titanium dioxide by-product titanium gypsum regeneration method according to claim 1 and 2, is characterized in that: when calcining in step b, and calcining top temperature controls at 170 ~ 220 DEG C, and this temperature lower calcination time controling was at 1 ~ 3 hour.
5. sulfate process titanium dioxide by-product titanium gypsum regeneration method according to claim 1 and 2, is characterized in that: require during levigate process in step c that granularity is greater than 200 orders.
6. sulfate process titanium dioxide by-product titanium gypsum regeneration method according to claim 1 and 2, it is characterized in that: in steps d, the granularity of described calcining natural gesso, calcining desulfurization gypsum powder, magnesia powder and silicon powder composite powder, Portland clinker is all greater than 200 orders.
7. sulfate process titanium dioxide by-product titanium gypsum regeneration method according to claim 2, is characterized in that: the length of vegetable fibre and paper fiber is 1 ~ 3mm.
8. sulfate process titanium dioxide by-product titanium gypsum regeneration method according to claim 1 and 2, is characterized in that: in step e, and the add-on of water is 80 ~ 110% of composite rear raw material gross weight.
9. sulfate process titanium dioxide by-product titanium gypsum regeneration method according to claim 1 and 2, is characterized in that: in step g, storing temperature controls at 80 ~ 120 DEG C, and baking time controlled at 12 ~ 36 hours.
10. titanium gypsum blockwork material, is characterized in that method obtains any one of claim 1 ~ 9.
CN201510296845.4A 2015-06-03 2015-06-03 Recycling method of sulfate process titanium dioxide by-product titanium gypsum Pending CN104944817A (en)

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Publication number Priority date Publication date Assignee Title
CN105399391A (en) * 2015-11-27 2016-03-16 武汉青江化工黄冈有限公司 Method for preparing gypsum plaster from titanium gypsum
CN105399390A (en) * 2015-11-27 2016-03-16 武汉青江化工黄冈有限公司 Method for preparing gypsum binder from titanium gypsum
CN105461245A (en) * 2015-11-30 2016-04-06 马鞍山泓宇材料科技有限公司 Titanium gypsum slurry dehydration method
CN107777960A (en) * 2016-08-31 2018-03-09 武春洋 A kind of industrial residue titanium gypsum building block and preparation method thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105399391A (en) * 2015-11-27 2016-03-16 武汉青江化工黄冈有限公司 Method for preparing gypsum plaster from titanium gypsum
CN105399390A (en) * 2015-11-27 2016-03-16 武汉青江化工黄冈有限公司 Method for preparing gypsum binder from titanium gypsum
CN105461245A (en) * 2015-11-30 2016-04-06 马鞍山泓宇材料科技有限公司 Titanium gypsum slurry dehydration method
CN107777960A (en) * 2016-08-31 2018-03-09 武春洋 A kind of industrial residue titanium gypsum building block and preparation method thereof

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