CN104692443A - Manufacturing method using 1,5 naphthalene disulfonic acid reactive mother solution to prepare calcium sulfate - Google Patents
Manufacturing method using 1,5 naphthalene disulfonic acid reactive mother solution to prepare calcium sulfate Download PDFInfo
- Publication number
- CN104692443A CN104692443A CN201510131516.4A CN201510131516A CN104692443A CN 104692443 A CN104692443 A CN 104692443A CN 201510131516 A CN201510131516 A CN 201510131516A CN 104692443 A CN104692443 A CN 104692443A
- Authority
- CN
- China
- Prior art keywords
- disulfonic acid
- naphthalene disulfonic
- percents
- calcium sulfate
- mother liquor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
Abstract
The invention discloses a manufacturing method using a 1,5 naphthalene disulfonic acid reactive mother solution to prepare calcium sulfate. The manufacturing method comprises the following steps, firstly, a 1,5 naphthalene disulfonic acid mother solution is added into a reaction still, the content of the mother solution is 1,5 naphthalene disulfonic acid with a concentration ranging from five percents to ten percents and sulfuric acid with a concentration ranging from 30 percents to 60 percents, calcium carbonate powder which is of 40 percents to 60 percents of the volume of the 1,5 naphthalene disulfonic acid mother solution is slowly added into the mother solution while stirring is carried out, and adding of the calcium carbonate powder stops when the pH reaches a value ranging from six to seven; secondly, water which is of 0.2 to 0.5 time of the volume of the 1,5 naphthalene disulfonic acid mother solution is added, stirring is carried out at a temperature ranging from 50 DEG C to 80 DEG C, and reaction is carried out for one hour to two hours, after the reaction is completed, the calcium sulfate is obtained after filter-pressing is carried out at a temperature ranging from 50 DEG C to 80 DEG C, the calcium sulfate content ranges from 63 percents to 70 percents, and the sulfur trioxide content in the calcium sulfate ranges from 37 percents to 42 percents; the mother solution is obtained after filter-pressing is carried out, and the 1,5 naphthalene disulfonic acid calcium content in the filter-pressed mother solution ranges from 20 percents to 30 percents. The method has the advantages that the technology is simple, the investment is little, and the produced mother solution can be recycled.
Description
Technical field
The invention belongs to chemical field, particularly utilize 1,5-naphthalene disulfonic acid reaction mother liquor to prepare the production method of calcium sulfate.
Background technology
Calcium sulfate can be used as cement raw material; As cement retarding agent; Gypsum.Chemical formula CaSO4.Molecular weight 136.14, oblique system, crystal is tabular, column, and aggregate is compact mass, threadiness, sheet, earthy or the kidney shape.Vitreous luster, is slightly soluble in water, is dissolved in hydrochloric acid.
Calcium sulfate is the raw material manufacturing cement, calcium sulphate hemihydrate and sulfuric acid.Weighting agent is used as in paint and paper industry.Agriculturally be used as chemical fertilizer, soil alkalinity can be reduced, improve soil function.Food grade with accessory substance (calcium fortified), peptizer, yeast food, dough conditioner, sequestrant, can also be used as texture strenghener, the stiffening agent of brewing water, the flavour enhancer etc. of wine in can.Because the Application and Development of its derived product increases gradually, the Application Areas of this product in chemical industry is constantly expanded.
Existing calcium sulfate production technology, is plaster of paris ore deposit Ex-all impurity, earth are formed through calcining abrasive dust, also has strip mining transformation also to have underground mining.Above technological system is complicated, and floor space is large; Cost is high, and one-time investment is large; Operation problem is more---and easily deposit due to byproduct CaSO4 and bond, so, easily cause system incrustation, blocking and wearing and tearing; Working cost is high, and high liquid/gas is very larger than the electricity brought, water cycle and consumption; The composition of desulfurated plaster is unstable; Waste resource; Production method is complicated and there is unsafe factor, is unfavorable for the physical and mental health of worker.
Summary of the invention
For above-mentioned the deficiencies in the prior art, the invention provides one and utilize 1,5-naphthalene disulfonic acid reaction mother liquor prepares calcium sulfate production method, the method utilizes the chemical waste liquid produced in 1,5-naphthalene disulfonic acid production process to produce as raw material, advanced simple, cost is low, easy to operate, produce waste liquid recycling, there is significant economic benefit and social benefit.
Technical scheme of the present invention is: one utilizes 1,5-naphthalene disulfonic acid reaction mother liquor to prepare the production method of calcium sulfate, comprises the following steps:
Step one: add 1,5-naphthalene disulfonic acid mother liquor in a kettle., its content is 1, the 5-naphthalene disulfonic acid of 5-10%, the sulfuric acid of 30-60%, this exothermic heat of reaction.Slowly add the Paris white of the 40-60% of 1,5-naphthalene disulfonic acid mother liquor amount under stirring, adjust during pH=6-7 and stop adding Paris white;
Step 2: add 1 again after adding, the water of 0.2-0.5 times of 5-naphthalene disulfonic acid mother liquor amount is in 50-80 DEG C of stirring reaction 1-2 hour, calcium sulfate is obtained in 50-80 DEG C of press filtration after having reacted, content is 63-70%, sulfur trioxide content 37-42% in this calcium sulfate, and press filtration mother liquor, in this press filtration mother liquor, 1,5-naphthalene disulfonic acid calcium contents is 20-30%;
Step 3: add 1 again in press filtration mother liquor step 2 obtained, 5-naphthalene disulfonic acid mother liquor, its content is 1 of 5-10%, 5-naphthalene disulfonic acid, the sulfuric acid of 30-60%, adds Paris white under stirring again, adjust pH=5-7, stir press filtration after 1-2 hour and obtain the calcium sulfate of content 63-70%, the sulfur trioxide content 37-42 in this calcium sulfate, and press filtration mother liquor.
Step 4: replaced by this press filtration mother liquor the water recycle added to utilize.
Advantageous effect of the present invention is: simple to operate, and occupation area of equipment is little; Equipment is simple, and invest less, the mother liquor of generation is capable of circulation to be applied mechanically, and whole production process does not produce waste water, and the product composition obtained is stablized.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment 1:
Step one: in a kettle. suction 2000kg 1, (its content is 1 to 5-naphthalene disulfonic acid mother liquor, 5-naphthalene disulfonic acid: 5-10%, sulfuric acid: 30-60%) and the water of 800kg, slowly Paris white is added under stirring, exothermic heat of reaction, stop when pH is 6-7 adding Paris white, the calcium carbonate added is about 800kg.Now temperature 60 C, is warmed up to 70 DEG C of insulation reaction;
Step 2: stir 2 hours repetition measurement pH value at 70 DEG C, react complete when pH=6 is constant;
Step 3: it is 2000kg and press filtration mother liquor that 60 DEG C of press filtrations obtain calcium sulfate tide product.The content now obtaining calcium sulfate is 67%, and the sulfur trioxide content of this calcium sulfate is 39.4%.
Embodiment 2:
Step one
The press filtration mother liquor that step 3 in embodiment 1 obtained is (now in mother liquor 1,5-naphthalene disulfonic acid calcium contents is 20-30%) suction reactor, (its content is 1,5-naphthalene disulfonic acid: 5-10% to 1, the 5-naphthalene disulfonic acid mother liquor of suction 2000kg again, sulfuric acid: 30-60%), slowly add Paris white under stirring, now do not need to add water again, exothermic heat of reaction, therefore do not need heating, adjust pH=6-7;
Step 2
Stop as pH=6-7 adding Paris white, now temperature is 50 DEG C, and in 50 DEG C of insulated and stirred, 1 hour repetition measurement pH value, when pH=6 value, press filtration obtains calcium sulfate tide product 2050kg and press filtration mother liquor, the calcium sulphate content obtained is 66%, and the sulfur trioxide content in this calcium sulfate is 38.8%.
Step 3
The press filtration mother liquor obtained in step 2 is continued recycle by embodiment 2 again.
Claims (1)
1. the production method utilizing 1,5-naphthalene disulfonic acid reaction mother liquor to prepare calcium sulfate, is characterized in that: comprise the following steps:
Step one: add 1,5-naphthalene disulfonic acid mother liquor in a kettle., its content is 1 of 5-10%, 5-naphthalene disulfonic acid, the sulfuric acid of 30-60%, slowly adds 1 under stirring, the Paris white of the 40-60% of 5-naphthalene disulfonic acid mother liquor amount, adjusts during pH=6-7 and stops adding Paris white;
Step 2: add 1 again, the water of 0.2-0.5 times of 5-naphthalene disulfonic acid mother liquor amount is in 50-80 DEG C of stirring reaction 1-2 hour, calcium sulfate is obtained in 50-80 DEG C of press filtration after having reacted, content is 63-70%, sulfur trioxide content 37-42% in this calcium sulfate, and press filtration mother liquor, in this press filtration mother liquor, 1,5-naphthalene disulfonic acid calcium contents is 20-30%;
Step 3: add 1 again in press filtration mother liquor step 2 obtained, 5-naphthalene disulfonic acid mother liquor, its content is 1 of 5-10%, 5-naphthalene disulfonic acid, the sulfuric acid of 30-60%, adds Paris white under stirring again, adjust pH=5-7, stir press filtration after 1-2 hour and obtain the calcium sulfate of content 63-70%, the sulfur trioxide content 37-42 in this calcium sulfate, and press filtration mother liquor;
Step 4: replaced by this press filtration mother liquor the water recycle added to utilize.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510131516.4A CN104692443A (en) | 2015-03-24 | 2015-03-24 | Manufacturing method using 1,5 naphthalene disulfonic acid reactive mother solution to prepare calcium sulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510131516.4A CN104692443A (en) | 2015-03-24 | 2015-03-24 | Manufacturing method using 1,5 naphthalene disulfonic acid reactive mother solution to prepare calcium sulfate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104692443A true CN104692443A (en) | 2015-06-10 |
Family
ID=53340062
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510131516.4A Pending CN104692443A (en) | 2015-03-24 | 2015-03-24 | Manufacturing method using 1,5 naphthalene disulfonic acid reactive mother solution to prepare calcium sulfate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104692443A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106241849A (en) * | 2016-06-27 | 2016-12-21 | 枣庄市泰瑞精细化工有限公司 | A kind of method utilizing the waste water producing naphthalenedisulfonic acid to prepare gypsum for cement |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1648291A (en) * | 2004-11-30 | 2005-08-03 | 上海耀华纳米科技有限公司 | Process for preparing whisker calcium sulfate |
| CN101029415A (en) * | 2007-01-23 | 2007-09-05 | 东北大学 | Production of non-metallic material calcium-sulfate whiskers |
| CN102030354A (en) * | 2010-10-18 | 2011-04-27 | 中蓝连海设计研究院 | Treatment method of waste sulfuric acid |
-
2015
- 2015-03-24 CN CN201510131516.4A patent/CN104692443A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1648291A (en) * | 2004-11-30 | 2005-08-03 | 上海耀华纳米科技有限公司 | Process for preparing whisker calcium sulfate |
| CN101029415A (en) * | 2007-01-23 | 2007-09-05 | 东北大学 | Production of non-metallic material calcium-sulfate whiskers |
| CN102030354A (en) * | 2010-10-18 | 2011-04-27 | 中蓝连海设计研究院 | Treatment method of waste sulfuric acid |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106241849A (en) * | 2016-06-27 | 2016-12-21 | 枣庄市泰瑞精细化工有限公司 | A kind of method utilizing the waste water producing naphthalenedisulfonic acid to prepare gypsum for cement |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102603219B (en) | Process for preparing high-activity semi-hydrated gypsum cementing material and gypsum product by aid of phosphorous gypsum | |
| EP3351507B1 (en) | Method for producing wet-process phosphoric acid and by-producing alpha-hemihydrate gypsum and high-purity and high-whiteness alpha-hemihydrate gypsum | |
| CN105174760B (en) | A kind of method that dihydrate gypsum prepares αsemiwatergypsum | |
| EP3351506B1 (en) | Method for producing phosphoric acid and by-producing alpha-hemihydrate gypsum by wet-process | |
| CN104876528B (en) | A kind of method that utilization lithium aluminium houghite prepares the early injection pulp material of dual liquid type | |
| CN103011642B (en) | Method for preparing high-strength alpha-type hemihydrate gypsum by utilizing calcium carbide sludge modified phosphogypsum with normal pressure hydrothermal method | |
| CN102515610B (en) | Aliphatic series high efficiency water reducing agent and preparation method thereof | |
| CN110128045A (en) | II type anhydrous gypsum fast hydration exciting agent of one kind and fast hydration method | |
| CN105154979B (en) | A kind of method for producing phosphoric acid by wet process by-product αsemiwatergypsum whisker and the high whiteness αsemiwatergypsum whisker of high-purity | |
| CN102557719A (en) | Production method of gypsum board | |
| CN106811801A (en) | A kind of preparation method of modified gypsum whisker | |
| CN105236778B (en) | A kind of production method of phosphoric acid by wet process by-product high-purity whiteness αsemiwatergypsum high and compound organic and inorganic fertilizer | |
| CN107056115A (en) | A kind of rush for ardealite based cementitious material coagulates type early strength agent and preparation method thereof | |
| CN104229854A (en) | Calcium chloride solution producing method | |
| CN104760976A (en) | Comprehensive utilization method of potassium-containing shale by microwave treatment | |
| CN103011641B (en) | Method for preparing high-activity alpha type hemihydrate gypsum cementing materials by using reaction of chlorine-alkali waste liquid treating ardealite | |
| CN107059134A (en) | A kind of method that crystal whisker of gypsum is prepared under normal pressure | |
| CN104828851B (en) | A kind of calcium sulphate dihydrate production method and process units | |
| CN106629806A (en) | Method for producing dihydrate gypsum from waste liquid in laterite nickel ore wet process | |
| CN103395817A (en) | Preparation method of high-purity anhydrous calcium sulfate | |
| CN104692443A (en) | Manufacturing method using 1,5 naphthalene disulfonic acid reactive mother solution to prepare calcium sulfate | |
| CN104692442B (en) | A kind of method utilizing mid low grade phosphate rock association calcium resource to prepare high-purity high-strength Gypsum Fibrosum | |
| CN108314342A (en) | A kind of method that phosphogypsum dihydrate prepares alpha type high-strength gypsum | |
| CN1221489C (en) | Process for preparing plastering gypsum | |
| CN102965722B (en) | By-product aqueous sodium persulfate solution micro emulsion method produces calcium sulfate whisker |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150610 |