CN102191021B - Preparation method for lignosulfonic acid iron and manganese salt - Google Patents
Preparation method for lignosulfonic acid iron and manganese salt Download PDFInfo
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- CN102191021B CN102191021B CN2011100789714A CN201110078971A CN102191021B CN 102191021 B CN102191021 B CN 102191021B CN 2011100789714 A CN2011100789714 A CN 2011100789714A CN 201110078971 A CN201110078971 A CN 201110078971A CN 102191021 B CN102191021 B CN 102191021B
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- FOGYNLXERPKEGN-UHFFFAOYSA-N 3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfopropyl)phenoxy]propane-1-sulfonic acid Chemical compound COC1=CC=CC(CC(CS(O)(=O)=O)OC=2C(=CC(CCCS(O)(=O)=O)=CC=2)OC)=C1O FOGYNLXERPKEGN-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title abstract description 22
- 229910052742 iron Inorganic materials 0.000 title abstract description 11
- 150000002696 manganese Chemical class 0.000 title abstract 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 18
- -1 lignosulfonic acid iron salt Chemical class 0.000 claims abstract description 13
- 239000012266 salt solution Substances 0.000 claims abstract description 8
- 238000009833 condensation Methods 0.000 claims abstract description 4
- 230000005494 condensation Effects 0.000 claims abstract description 4
- 230000001590 oxidative effect Effects 0.000 claims abstract description 4
- 150000003839 salts Chemical class 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 239000001117 sulphuric acid Substances 0.000 claims description 16
- 235000011149 sulphuric acid Nutrition 0.000 claims description 16
- 239000004575 stone Substances 0.000 claims description 15
- 239000012286 potassium permanganate Substances 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 10
- 239000007788 liquid Substances 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 9
- 238000006073 displacement reaction Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 4
- 239000011575 calcium Substances 0.000 abstract description 4
- 229910052791 calcium Inorganic materials 0.000 abstract description 4
- 238000001914 filtration Methods 0.000 abstract description 4
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 abstract description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract description 3
- 229910001424 calcium ion Inorganic materials 0.000 abstract description 3
- 229910052748 manganese Inorganic materials 0.000 abstract description 3
- 239000011572 manganese Substances 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract 2
- 238000002156 mixing Methods 0.000 abstract 1
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 10
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 9
- 239000002699 waste material Substances 0.000 description 8
- 238000005553 drilling Methods 0.000 description 7
- 238000004537 pulping Methods 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 229920001732 Lignosulfonate Polymers 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000002950 deficient Effects 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 4
- 229920005610 lignin Polymers 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 235000003891 ferrous sulphate Nutrition 0.000 description 3
- 239000011790 ferrous sulphate Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 3
- 150000002978 peroxides Chemical class 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- JXLHNMVSKXFWAO-UHFFFAOYSA-N azane;7-fluoro-2,1,3-benzoxadiazole-4-sulfonic acid Chemical compound N.OS(=O)(=O)C1=CC=C(F)C2=NON=C12 JXLHNMVSKXFWAO-UHFFFAOYSA-N 0.000 description 2
- LVGQIQHJMRUCRM-UHFFFAOYSA-L calcium bisulfite Chemical compound [Ca+2].OS([O-])=O.OS([O-])=O LVGQIQHJMRUCRM-UHFFFAOYSA-L 0.000 description 2
- 235000010260 calcium hydrogen sulphite Nutrition 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920005615 natural polymer Polymers 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 229920001864 tannin Polymers 0.000 description 2
- 235000018553 tannin Nutrition 0.000 description 2
- 239000001648 tannin Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical class [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- JHWIEAWILPSRMU-UHFFFAOYSA-N 2-methyl-3-pyrimidin-4-ylpropanoic acid Chemical compound OC(=O)C(C)CC1=CC=NC=N1 JHWIEAWILPSRMU-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- 235000018783 Dacrycarpus dacrydioides Nutrition 0.000 description 1
- 244000288671 Dacrycarpus dacrydioides Species 0.000 description 1
- 235000005456 Pinus sylvestris var mongolica Nutrition 0.000 description 1
- 241000114025 Pinus sylvestris var. mongolica Species 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- UPHIPHFJVNKLMR-UHFFFAOYSA-N chromium iron Chemical compound [Cr].[Fe] UPHIPHFJVNKLMR-UHFFFAOYSA-N 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- SUOFREPYJDSUTJ-UHFFFAOYSA-N iron sulfurous acid Chemical compound [Fe].S(O)(O)=O SUOFREPYJDSUTJ-UHFFFAOYSA-N 0.000 description 1
- 239000003077 lignite Substances 0.000 description 1
- 235000019357 lignosulphonate Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000003265 pulping liquor Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Paper (AREA)
Abstract
The invention provides a preparation method for lignosulfonic acid iron and manganese salt. The method comprises the following steps: (a) mixing lignosulfonic acid, iron oxide, dilute sulfuric acid and oxidizing agent to obtain lignosulfonic acid iron salt solution; (b) adding oxide containing manganese into the lignosulfonic acid iron salt solution to carry out oxidative condensation; (c) drying the resultant solution to obtain lignosulfonic acid iron and manganese salt. According to the preparation method for lignosulfonic acid iron and manganese salt provided in the invention, lignosulfonic acid is taken as raw material, calcium ion content is reduced, filtration and calcium removal are avoided, material loss is reduced, and the operation of preparing displacement liquid is omitted. Compared with traditional preparation method, the method provided in the invention has simple operation and is labour-saving and time-saving.
Description
Technical field
The present invention relates to slurry thinner fields such as geological drilling, petroleum drilling, be specifically related to a kind of preparation method of lignosulfonic acid ferrimanganic salt.
Background technology
Along with the development of petroleum industry, the polymer organic treatment agent is widely used in drilling fluid, and property of drilling fluid is regulated by treatment agent, and the current most of treatment agent that uses is an organic polymer.The drilling fluid organic agent has natural polymer at present, like tannin, tannin extract, brown coal, spiceleaf powder, dog bone powder etc.; Modified natural polymers is like feero-chromo-lignosulfonate (FCLS), sodium carboxymethyl-cellulose (Na-CMC); Synthetic polymer is like acrylic amide, sulfonated phenol formaldehyde resin etc.
The fifties in last century, feero-chromo-lignosulfonate is used for drilling fluid, the widespread use because anti-salt property and resistance toheat are superior.The chromium-iron lignosulfonate lignosulfonic acid is that raw material adds ferrous sulfate, the sodium dichromate 99 reaction forms with the lignosulfite that contains lignosulfonic acid.
But chromium is heavy metal element, can serious environment pollution, be prone to be absorbed after the human body contact, and carcinogenic danger is arranged, so feero-chromo-lignosulfonate is restricted as the use of drilling diluter.Low chromium and Chrome-free product constantly occur, like the XPA of sulfonated lignin, and the boride of lignosulfonic acid, lignosulfonic acid molysite, lignosulfonic acid manganese salt, lignosulfonic acid ferrimanganic salt.Wherein lignosulfonic acid ferrimanganic salt technology is ripe, and excellent performance is used widely.
The method of existing lignosulfonic acid ferrimanganic salt is a main raw material with calcium lignin sulphonate, sulfurous acid iron, sulfuric acid, ydrogen peroxide 50, potassium permanganate, obtains lignosulfonic acid ferrimanganic salt through steps such as displacement liquid preparation, displacement, filtration, potassium permanganate oxidations.Calcium contents in the calcium lignin sulphonate is between 6%～7%.The preparation process need is through filtering operation together, and also will prepare displacement liquid, and the preparation process wastes time and energy.
Summary of the invention
The problem that the present invention solves is to provide a kind of preparation method of lignosulfonic acid ferrimanganic salt, and operation is simple, need not to filter and prepare displacement liquid, and is time saving and energy saving.
In order to solve the problems of the technologies described above, technical scheme of the present invention is:
A kind of preparation method of lignosulfonic acid ferrimanganic salt may further comprise the steps:
A) lignosulfonic acid, red stone, dilute sulphuric acid and oxygenant are mixed, obtain the lignosulfonic acid iron salt solutions;
B) in the lignosulfonic acid iron salt solutions, add manganiferous oxide compound and carry out oxidative condensation;
C) gained solution is dry, obtain lignosulfonic acid ferrimanganic salt.
As preferably, said a) in the mass ratio of lignosulfonic acid and red stone be 4～10: 1.
As preferably, said a) in the mass percent concentration of dilute sulphuric acid below 10%, the mass ratio of lignosulfonic acid and said dilute sulphuric acid is 0.8～2: 1.
As preferably, said a) in oxygenant be in the vitriol oil, nitric acid or the hydrochloric acid one or more.
As preferably, the quality of said oxygenant be said lignosulfonic acid quality 3%～5%.
As preferably, said temperature of reaction a) is 50 ℃～90 ℃.
As preferably, said b) manganiferous oxide compound is one or more in manganese oxide, Manganse Dioxide, manganic oxide, the potassium permanganate in.
As preferably, said b) manganiferous oxide compound is a potassium permanganate in.
As preferably, the quality of said manganiferous oxide compound be said lignosulfonic acid quality 2%～4%.
As preferably, said b) temperature of reaction is 70 ℃～100 ℃.
The preparation method of a kind of lignosulfonic acid ferrimanganic salt provided by the invention uses lignosulfonic acid to be raw material, reduces calcium ion content; Need not filter deliming, reduce loss of material, and save the operation of preparation displacement liquid; Compare with the traditional preparation process method, operation is simpler, and is time saving and energy saving.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment the preferred embodiment of the invention is described, describe just to further specifying feature and advantage of the present invention but should be appreciated that these, rather than to the restriction of claim of the present invention.
The preparation method of lignosulfonic acid ferrimanganic salt provided by the invention may further comprise the steps:
A) lignosulfonic acid, red stone, dilute sulphuric acid and oxygenant are mixed, obtain the lignosulfonic acid iron salt solutions.
Lignosulfonic acid and red stone can use the waste liquid that contains lignosulfonic acid and the sub product red stone that produce in the sulfurous acid pulping process to react, and so also can handle pulping waste liquor simultaneously, recycle xylogen wherein.Acid sulfurous acid pulping waste liquor preferably uses with the spent pulping liquor of timber as raw material, like pinus sylvestris var. mongolica, kahikatea etc.In the pulping process; Sulfurous iron ore burning back produces sulfurous gas through absorbing; Obtain calcium bisulfite, re-use calcium bisulfite and xylogen is carried out sulfonation promptly obtain the lignosulfonic acid calcium salt, and the lignosulfonic acid calcium salt changes into lignosulfonic acid under acidic conditions; Therefore contain the lignosulfonic acid that can utilize again in a large number in the acid sulfurous acid pulping waste liquor, sulfurous iron ore burning simultaneously also produces the by product red stone.Therefore acid sulfurous acid pulping waste liquor that slurrying is produced and red stone are as raw material of the present invention.The mass ratio of lignosulfonic acid and red stone is 4～10: 1.
The mass percent concentration of dilute sulphuric acid is preferably below 10%, and the mass ratio of reaction raw materials lignosulfonic acid and this dilute sulphuric acid is for can be 0.8～2: 1.The dilute sulphuric acid that produces in the time of equally also can utilizing acid sulfurous acid pulping waste liquor to concentrate reacts.The adding quality of oxygenant be lignosulfonic acid quality 3%～5%, can select in the vitriol oil, nitric acid or the hydrochloric acid one or more for use.
This step reaction is preferably carried out under 50 ℃～90 ℃.
Can earlier red stone, dilute sulphuric acid and oxygenant be mixed during production, after question response is complete, adds lignosulfonic acid again and react, obtain the lignosulfonic acid molysite.Also can be earlier with lignosulfonic acid with after red stone mixes, add dilute sulphuric acid again and oxygenant reacts.
B) in the lignosulfonic acid iron salt solutions, add manganiferous oxide compound and carry out oxidative condensation.The quality of manganiferous oxide compound be the reactant lignosulfonic acid quality 2%～4%, can select in manganese oxide, Manganse Dioxide, manganic oxide, the potassium permanganate one or more for use, more preferably use potassium permanganate.
This step reaction is preferably carried out under 70 ℃～100 ℃.
C) gained solution is dry, promptly obtain lignosulfonic acid ferrimanganic product salt.
Embodiment 1:
Select for use the sulfurous acid pulp-making waste-water as raw material,, the sulfurous acid pulp-making waste-water is concentrated, obtain mass percent and be 45% lignosulfonic acid liquid concentrator for reducing floor space, pH value 1.8, calcareous amount content is less than 3.0%.
In reaction kettle, add 100 kilograms of red stone, the dilute sulphuric acid of 500 kilograms of recovery (producing when the sulfurous acid pulp-making waste-water concentrates), the dilute sulphuric acid mass concentration is 8%, adds 20 kilograms of vitriol oils again, is warming up to 60 ℃ of reactions 1 hour, the red stone total overall reaction is complete.Add 1000 kilograms of above-mentioned sulfomethylated lignin acid solutions, reaction is 30 minutes under 85 ℃ of-90 ℃ of conditions, obtains the lignosulfonic acid ferrous solution.The pH value of solution value is between 2.7, and all iron content is 6.8%.
Then, 15% solution that contains 60 kilograms of potassium permanganate 95 ℃ of addings.Insulation reaction 30 minutes gets lignosulfonic acid ferrimanganic salts solution, the spray-dried granular product that obtains.Through detecting, product moisture is less than 8.0%, manganese mass content 1.7%, and potassium mass content 1.2%, weight of iron content 6.8%, the water-insoluble quality is less than 2.5%, pH value of solution value 3.4.
Embodiment 2:
The sulfurous acid pulp-making waste-water is concentrated, obtain mass percent and be 48% lignosulfonic acid liquid concentrator, pH value 1.5, calcareous amount content is less than 3.0%.
In reaction kettle, add 1800 kilograms, 100 kilograms red stone of sulfomethylated lignin acid solution, add the dilute sulphuric acid (the dilute sulphuric acid mass concentration is 8%) of 500 kilograms of recovery, 40 kilograms of vitriol oils again, reaction is 30 minutes under 90 ℃ of conditions, obtains the lignosulfonic acid ferrous solution.The pH value of solution value is between 2.5-3.0, and full weight of iron content is 6.8%.
Then, 15% solution that contains 230 kilograms of potassium permanganate 85 ℃ of addings.Insulation reaction 30 minutes.Get lignosulfonic acid ferrimanganic salts solution, the spray-dried granular product that obtains.Through detecting, product moisture is less than 8.0%; Manganese content 2.4%; Potassium content 1.7%; Iron level 6.7%; Water-insoluble is less than 2.5%; Solution pH value 3.7.
Comparative example:
Earlier sulfuric acid is added in the entry, and then add ferrous sulfate, in the mixed solution of sulfuric acid and ferrous sulfate, add ydrogen peroxide 50 again, it is subsequent use to be mixed with displacer.
The displacer that adding prepares in paper pulp waste is heated to 80 ℃ and reacts, and obtains a defective material.
Then potassium permanganate is heated in 50 ℃ the water, is warming up to 85 ℃ then, fully stir, the preparation potassium permanganate solution.
React in the aforementioned defective material that obtains of potassium permanganate solution adding with preparation, be heated to 80 ℃, and insulation 20min, obtaining two defective materials, the pH value of two defective materials is controlled at 2.5～3.0, can process the dry powder finished product through spraying drying then.
Existing preparation method compares in the embodiment of the invention 1 and 2 the method for preparing lignosulfonic acid ferrimanganic salt and the comparative example, and is as shown in table 1:
The preparation method of table 1 lignosulfonic acid ferrimanganic of the present invention salt and the comparison of prior art
Preparing method of the present invention uses lignosulfonic acid to be raw material, reduces calcium ion content, need not to use ydrogen peroxide 50, and save the preparation displacement liquid, carry out replacement(metathesis)reaction, and filtering operation, the preparation process is more time saving and energy saving.
The lignosulfonic acid ferrimanganic salt of embodiment 1 and 2, comparative example preparation is compared, and the result is as shown in table 2:
The product comparative result of table 2 embodiment of the invention and comparative example
Data presentation in the table 2, the lignosulfonic acid ferrimanganic salt of the present invention's preparation is compared with the lignosulfonic acid ferrimanganic salt of prior art for preparing, pH and all iron content basically identical, the value of R600, R300 and YP/PV is less, and product quality is higher.
More than the preparation method of a kind of lignosulfonic acid ferrimanganic salt provided by the present invention has been carried out detailed introduction.Used concrete example among this paper principle of the present invention and embodiment are set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
Claims (3)
1. the preparation method of a lignosulfonic acid ferrimanganic salt is characterized in that, may further comprise the steps:
A) lignosulfonic acid, red stone, dilute sulphuric acid and oxygenant are mixed, obtain the lignosulfonic acid iron salt solutions; The mass ratio of lignosulfonic acid and red stone is 4～10: 1; The mass percent concentration of said dilute sulphuric acid is below 10%, and the mass ratio of lignosulfonic acid and said dilute sulphuric acid is 0.8～2: 1; Said oxygenant is one or more in the vitriol oil, nitric acid or the hydrochloric acid, the quality of said oxygenant be said lignosulfonic acid quality 3%～5%;
B) in the lignosulfonic acid iron salt solutions, add potassium permanganate and carry out oxidative condensation, the quality of potassium permanganate be said lignosulfonic acid quality 2%～4%;
C) gained solution is dry, obtain lignosulfonic acid ferrimanganic salt.
2. preparation method according to claim 1 is characterized in that, said temperature of reaction a) is 50 ℃～90 ℃.
3. preparation method according to claim 1 is characterized in that, said b) temperature of reaction be 70 ℃～100 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1404912A (en) * | 2002-11-08 | 2003-03-26 | 华南理工大学 | Modified lignin sulfosalt dispersant of water coal slurry |
| CN101624517A (en) * | 2009-07-29 | 2010-01-13 | 牡丹江市红林化工有限责任公司 | Ferrimanganic lignosulfonate diluent agent for drilling fluid and preparation process thereof |
| CN101759725A (en) * | 2010-01-27 | 2010-06-30 | 延边石岘白麓纸业股份有限公司 | Production method of chrome-free lignosulfonate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AR039786A1 (en) * | 2003-05-02 | 2005-03-02 | Jasinski Ricardo | ADDITIVE FOR PERFORATION FLUIDS |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1404912A (en) * | 2002-11-08 | 2003-03-26 | 华南理工大学 | Modified lignin sulfosalt dispersant of water coal slurry |
| CN101624517A (en) * | 2009-07-29 | 2010-01-13 | 牡丹江市红林化工有限责任公司 | Ferrimanganic lignosulfonate diluent agent for drilling fluid and preparation process thereof |
| CN101759725A (en) * | 2010-01-27 | 2010-06-30 | 延边石岘白麓纸业股份有限公司 | Production method of chrome-free lignosulfonate |
Non-Patent Citations (2)
| Title |
|---|
| 张洁.木质素钻井液添加剂.《西安石油学院学报》.1990,第5卷(第3期),60-64. * |
| 王中华等.国内钻井液用改性木质素类处理剂研究与应用.《精细石油化工进展》.2009,第10卷(第4期),19-22. * |
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