CN105385490A - Metal cutting emulsion prepared from coarse tall oil residues and preparation method thereof - Google Patents
Metal cutting emulsion prepared from coarse tall oil residues and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a metal cutting emulsion prepared from coarse tall oil residues and a preparation method thereof. The preparation method comprises the following steps: (1) neutralizing coarse tall oil residues; (2) separating coarse tall oil from the residues; (3) preparing coarse tall oil amide; (4) preparing metal cutting emulsion from coarse tall oil amide and other components. The tall oil amide obtained by the method mentioned above is compounded with base oil, a stabilizing agent, an antifoaming agent, a bactericide, an emulsifying agent, and deionized water according to a certain ratio, and then the mixture is emulsified to obtain stable metal cutting emulsion. The metal cutting emulsion prepared from coarse tall oil residues is subjected to anticorrosion performance and antirust performance detections that meet the national standards. The anticorrosion performance reaches the national B standard, and the antirust performance reaches the national A standard. The method has the advantages that the operation is convenient and simple, the environment is protected, the discharge of wastes is reduced, at the same time, the profits of enterprises are increased, and the cost is reduced.
Description
Technical field
The invention belongs to pine papermaking byproduct comprehensive and utilize technical field, relate to a kind of metal cutting emulsion utilizing the thick tall oil waste residue of pine pulping byproducts to prepare and preparation method thereof.
Background technology
The pine aboundresources such as south China Pinus massoniana Lamb, are commonly used for the starting material of pulping and paper-making.China, in recent years along with expanding economy, is that the pulping and paper-making industry of raw material is developed rapidly with pine.Containing compositions such as rosin, xylogen, Mierocrystalline cellulose, hemicelluloses in pine; in pine alkaline cooking pulping process; produce a large amount of by products; as tall oil (also known as tall oil), sulfate turpentine, alkali lignin (black liquid) etc.; comprehensively effectively utilize by product; both can economize on resources, protection of the environment, also can improve Business Economic Benefit and social environment.
In the alkaline process taking pine as raw material or kraft process digestion process, grease in pine and resinous principle are by saponification and the sodium salt forming lipid acid and resinous acid is dissolved in black liquor, neutral oil is also drawn out of and is dissolved in soap lye simultaneously, Here it is sulfate soap (tall oil containing 50-55%wt), xylogen is then converted into alkali lignin and is dissolved in black liquor, as spumescence, aterrimus cacodorous sulfate soap just float over above black liquor, black liquor is when simmer down to solids content 23%-32%, put into large storage tank, now hydrophilic resin acid soaps, fatty acid soaps is precipitated, oil-soluble unsaponifiables is also extracted out, float to black liquor top and form Black liquor soap layer, namely saponified recovery storage is obtained sulfate soap.
The separation and Extraction of sulfate soap compound has settled process, inflation process and centrifuging etc.There is not a large amount of foam because of its production process in settled process, easy and simple to handle, stable, efficiency is high, need not another oil (gas) filling device and being widely adopted.Saponifiedly after storagetank standing separation, be sent to rinse bath together with washings, alkaline washings can remove the lignin of saponified middle 60-80% and the fiber of about 50% and impurity effectively.Washedly in rinse bath be saponifiedly supplied to acidification system again.Saponified and sour in reactor reaction after, resolve into the components such as thick tall oil, alkali lignin, fiber and gypsum, discharge H simultaneously
2s and CO
2gas, reactor upper strata is then the thick tall oil that purity is higher, and also referred to as tall oil, lower floor is spent acid, waste water and solid sediment etc., and middle layer is the mixture containing compositions such as tall oil, alkali lignin and neutral unsaponifiables, i.e. thick tall oil waste residue.According to different pulping process and raw material, in the thick tall oil waste residue of gained, thick tall oil is different with the content of alkali lignin, in the thick tall oil waste residue of general dryness, thick tall oil content is at 40%-70%, and alkali lignin content is at 15%-40%, and all the other are neutral unsaponifiables.
Thick tal fibre main body of oil is resinous acid, lipid acid and neutrals, can obtain starex acid, floating oil fatty acid, tall oil pitch, distillation oil slick and hair oil after being separated, and is one of three large sources of sylvic acid and lipid acid.If carry out refining or further tall oil isolated the product such as sylvic acid, lipid acid, then can obtain utilizing more widely.
Starex acid: the structure of starex acid is similar to gum resin, and purposes and gum resin are substantially identical.Be mainly used in the departments such as glue used in paper-making, soap, ink, paint, coating, resin.If be processed into modified rosin or starex derivative further, its Application Areas will be expanded.
Floating oil fatty acid: main component is oleic acid and linolic acid, is widely used in softening agent, liquid soap, synthetic detergent, defoamer etc.
Tall oil pitch forms primarily of high boiling neutrals, except for except the departments such as tackiness agent, ink, paint, coating, also can extract β-sitosterol and replace cholest acid for the manufacture of various arteriosclerosis medicine and VITAMIN etc.
The present invention is directed to the composition of thick tall oil waste residue, the preparation of neutralizing treatment, tall oil acid amides, the separation of tall oil acid amides, the method such as compound and emulsification is taked to prepare metal cutting emulsion to high oily waste residue, through meeting the detection of national standard, prepared cutting good emulsion stability, corrosion resistance reaches national B grade standard, and rustless property reaches national A grade standard, can meet the needs that the metals such as iron, steel and copper are anticorrosion and antirust in cutting process.
By above-mentioned utilization, the economic benefit of waste residue can be improved significantly, eliminate the pollution to environment, have great society and economic implications to the recycle of promotion resource, the Sustainable development of realization society.
Summary of the invention
Technical problem to be solved by this invention is the waste residue after the thick tall oil of by product after utilizing pine slurrying is produced is raw material; preparation has the metal cutting emulsion of higher economic worth and the market requirement; reduce discharge and the protection of the environment of waste, enterprise's productive profit can be improved simultaneously, reduce costs.
In order to solve the problems of the technologies described above, the method for metal cutting emulsion prepared by the thick tall oil waste residue of utilization provided by the invention, adopts following steps:
(1) neutralizing treatment of thick tall oil waste residue: first according to the pH value of liquid in waste residue, add that appropriate basic solution carries out stirring, neutralization reaction, the liquid pH value controlling to produce is slightly acidic, leaves standstill, then remove lower floor's liquid, obtain thick tall oil waste residue after treatment;
(2) thick tal fibre oil separating: add organic solvent in the thick tall oil waste residue obtained after above-mentioned steps (1) process, after abundant stirring and dissolving, filter cleaner, then leave standstill, be separated removing water layer, obtain thick tall oil organic solution;
(3) preparation of thick tall oil acid amides: in the thick tall oil organic solution that above-mentioned steps (2) obtains, add the organic amine of requirement, mix, temperature reaction, underpressure distillation removing organic solvent again, cooling obtains viscous liquid, is thick tall oil acid amides finished product;
(4) the thick tall oil acid amides preparing metal obtained in above-mentioned steps (3) is utilized to cut emulsion.
Source and the feature of the thick tall oil waste residue described in above-mentioned steps (1) are: contained grease and resin are converted into saponified in alkaline cooking process, be dissolved in black liquor, pass through enrichment process, saponifiedly float on black liquor liquid level, separated and collected is saponified, then washs with washings, remove saponified in part lignin, fiber and other impurity, and then carry out acidification reaction, be separated by standing sedimentation, upper strata is the thick tall oil that alkali lignin content is very low; Middle layer is then the mixolimnion of thick tall oil and alkali lignin, i.e. thick tall oil waste residue, and lower floor is spent acid solution; In the thick tall oil waste residue of gained, thick tall oil content is 40-70%, and alkali lignin content is 15-40%, and all the other are neutral unsaponifiables.
Step (1) neutralization reaction alkali lye used comprises: the solution of sodium hydroxide or sodium carbonate or ammoniacal liquor or trolamine.
Step (1) the neutralization reaction time is 0.5-1.0h, and the liquid pH value controlling to produce is 5.5-6.5, leaves standstill 2-4h, then removes lower floor's liquid, obtains thick tall oil waste residue after treatment.
The organic solvent dissolving thick tall oil waste residue described in step (2) comprises benzene, toluene or dimethylbenzene.
In thick tall oil organic solution step (2) obtained in step (3), add the organic amine of requirement, the mass ratio of the organic amine quality added and the thick tall oil waste residue of over dry is 0.08-0.50, mixes.
Organic amine described in step (3) comprises containing C
2~ C
6any one or several in the primary amine of carbochain, secondary amine, diamines, triamine, thanomin.
At N in step (3)
2be warming up to 120-160 DEG C under protective condition, reaction 2-5h, then forward in water distilling apparatus by solution, underpressure distillation removing organic solvent, under room temperature, cooling obtains viscous liquid, is thick tall oil acid amides finished product.
Step (4) utilizes in step (3) the thick tall oil acid amides obtained, with the base oil of certain mass ratio, stablizer, defoamer, sterilant, emulsifying agent, deionized water 40 DEG C-70 DEG C carry out composite, dissolve and emulsification 1-3h, finally obtain metal cutting emulsion.
The present invention utilizes thick tall oil waste residue to prepare metal cutting emulsion and solves the waste residue produced in thick tall oil producing process and be difficult to because its main component character is close be effectively separated and cause the problem that thick tall oil waste residue at present is not yet effectively separated and utilizes.Utilize the feature that in thick tall oil waste residue, thick tall oil content is higher, by the neutralizing treatment of thick tall oil waste residue, thick tal fibre oil separating, the preparation of your oleylamide thick, composite with means such as emulsifications, obtain corrosion resistance and reach the metal cutting emulsion that national B grade standard and rustless property reach national A grade standard and good stability, iron can be met, steel, aluminium, the needs that the metallic substance such as steel alloy and copper is anticorrosion and antirust in cutting process, thus achieve the direct utilization of tall oil in this waste residue, preparation has the metal cutting emulsion of higher economic worth and the market requirement, to the economic worth and the enterprise profit that improve waste residue, reduce waste residue to the impact of environment simultaneously, there is positive meaning.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and non-formation limitation of the present invention.
Embodiment 1:
(1) neutralization of thick tall oil waste residue and saponification, first according to the pH value of liquid in waste residue, add that appropriate basic solution carries out stirring in room temperature, neutralization reaction, time is about 0.5h, in control and the pH value of waste liquid be about 6.0, leave standstill 3h, then remove lower floor's liquid, obtain treated thick tall oil waste residue;
(2) thick tal fibre oil separating: add toluene in the thick tall oil waste residue obtained after above-mentioned (1) process, after abundant stirring and dissolving, filter cleaner, then leave standstill 2h, be separated removing water layer, obtain thick tall oil toluene solution;
(3) preparation of thick tall oil acid amides: in the thick tall oil toluene solution that above-mentioned (2) obtain, add the quadrol of requirement, the mass ratio of the quadrol quality added and the thick tall oil waste residue of over dry is 0.10, mixes, at N
2be warming up to 150 DEG C under protective condition, reaction 4h, then forward in water distilling apparatus by solution, underpressure distillation removing toluene, under room temperature, cooling obtains viscous liquid, is thick tall oil acid amides finished product.
(4) preparation of metal cutting emulsion: utilize the thick tall oil acid amides that above-mentioned steps (3) obtains, with the thick tall oil acid amides of mass percent 18.89%, 20.46% base oil, 4.79% boric acid, 0.50% dimethyl silicone oil, 10.0% trisodium phosphate, 1.54% polyoxyethylene glycol, 0.48% KF88, the OP-10 of 5.19%, the sodium laurylsulfonate of 9.99% and surplus deionized water carry out Solution and emulsification about 1h at about 60 DEG C, obtain water-in-oil-type metal cutting emulsion.
Embodiment 2:
(1) neutralizing treatment of thick tall oil waste residue: first according to the pH value of liquid in waste residue, add that appropriate basic solution carries out stirring in room temperature, neutralization reaction, time is about 0.5h, in control and the pH value of waste liquid be about 6.0, leave standstill 3h, then remove lower floor's liquid, obtain treated thick tall oil waste residue;
(2) thick tal fibre oil separating: add dimethylbenzene as solvent in the thick tall oil waste residue obtained after above-mentioned (1) process, after abundant stirring and dissolving, filter cleaner, then leave standstill 2h, be separated removing water layer, obtain the xylene solution of thick tall oil;
(3) preparation of thick tall oil acid amides: in the thick tall oil xylene solution that above-mentioned (2) obtain, add the quadrol of requirement, the mass ratio of the quadrol quality added and the thick tall oil waste residue of over dry is 0.10, mixes, at N
2be warming up to 150 DEG C under protective condition, reaction 4h, then forward in water distilling apparatus by solution, underpressure distillation is except removal xylene, and under room temperature, cooling obtains viscous liquid, is thick tall oil acid amides finished product.
(4) preparation of metal cutting emulsion, utilize the thick tall oil acid amides that above-mentioned steps (3) obtains, with the thick tall oil acid amides of mass percent 18.89%, 20.46% base oil, 4.79% boric acid, 0.50% dimethyl silicone oil, 10.0% trisodium phosphate, 1.54% polyoxyethylene glycol, 0.48% KF88, the OP-10 of 5.19%, the petroleum sodium sulfonate of 9.99% and surplus deionized water carry out Solution and emulsification about 1h at about 60 DEG C, obtain water-in-oil-type metal cutting emulsion.
Embodiment 3:
(1) neutralizing treatment of thick tall oil waste residue: first according to the pH value of liquid in waste residue, add that appropriate basic solution carries out stirring in room temperature, neutralization reaction, time is about 0.5h, in control and the pH value of waste liquid be about 6.0, leave standstill 3h, then remove lower floor's liquid, obtain treated thick tall oil waste residue;
(2) thick tal fibre oil separating: add dimethylbenzene as solvent in the thick tall oil waste residue obtained after above-mentioned (1) process, after abundant stirring and dissolving, filter cleaner, then leave standstill 2h, be separated removing water layer, obtain the xylene solution of thick tall oil;
(3) preparation of thick tall oil acid amides: in the thick tall oil xylene solution that above-mentioned (2) obtain, add the diethylenetriamine of requirement, the mass ratio of the diethylenetriamine quality added and the thick tall oil waste residue of over dry is 0.18, mixes, at N
2be warming up to 150 DEG C under protective condition, reaction 3h, then forward in water distilling apparatus by solution, underpressure distillation is except removal xylene, and under room temperature, cooling obtains viscous liquid, is thick tall oil acid amides finished product.
(4) preparation of metal cutting emulsion, utilize the thick tall oil acid amides that above-mentioned steps (3) obtains, with the thick tall oil acid amides of mass percent 18.89%, the base oil of 20.46%, boric acid, the dimethyl silicone oil of 0.50%, trisodium phosphate, the polyoxyethylene glycol of 1.54%, the KF88 of 0.48% of 10.0% of 4.79%, the deionized water of the OP-10 of 5.19%, the petroleum sodium sulfonate of 9.99% and surplus carries out Solution and emulsification about 1h at about 60 DEG C, obtains water-in-oil-type metal cutting emulsion.
Embodiment 4:
(1) neutralizing treatment of thick tall oil waste residue: first according to the pH value of liquid in waste residue, add that appropriate basic solution carries out stirring in room temperature, neutralization reaction, time is about 1.0h, in control and the pH value of waste liquid be about 6.0, leave standstill 2-4h, then remove lower floor's liquid, obtain treated thick tall oil waste residue;
(2) thick tal fibre oil separating: add dimethylbenzene as solvent in the thick tall oil waste residue obtained after above-mentioned (1) process, after abundant stirring and dissolving, filter cleaner, then leave standstill 1-2h, be separated removing water layer, obtain the xylene solution of thick tall oil;
(3) preparation of thick tall oil acid amides: in the thick tall oil xylene solution that above-mentioned (2) obtain, add the diethanolamine of requirement, the mass ratio of the diethanolamine quality added and the thick tall oil waste residue of over dry is 0.19, mixes, at N
2be warming up to 160 DEG C under protective condition, reaction 5h, then forward in water distilling apparatus by solution, underpressure distillation is except removal xylene, and under room temperature, cooling obtains viscous liquid, is thick tall oil acid amides finished product.
(4) preparation of metal cutting emulsion, utilize the thick tall oil acid amides that above-mentioned steps (3) obtains, with the thick tall oil acid amides of mass percent 18.89%, 20.46% base oil, 4.79% boric acid, 0.50% dimethyl silicone oil, 10.0% trisodium phosphate, 1.54% polyoxyethylene glycol, 0.48% KF88, the OP-10 of 5.19%, the petroleum sodium sulfonate of 9.99% and surplus deionized water carry out Solution and emulsification about 1h at about 60 DEG C, obtain water-in-oil-type metal cutting emulsion.
Embodiment 5:
(1) neutralizing treatment of thick tall oil waste residue: first according to the pH value of liquid in waste residue, add that appropriate basic solution carries out stirring in room temperature, neutralization reaction, time is about 0.5h, in control and the pH value of waste liquid be about 6.0, leave standstill 3h, then remove lower floor's liquid, obtain treated thick tall oil waste residue;
(2) thick tal fibre oil separating: add dimethylbenzene as solvent in the thick tall oil waste residue obtained after above-mentioned (1) process, after abundant stirring and dissolving, filter cleaner, then leave standstill 2h, be separated removing water layer, obtain thick tall oil xylene solution;
(3) preparation of thick tall oil acid amides: in the thick tall oil xylene solution that above-mentioned (2) obtain, add the diethylenetriamine of requirement, the mass ratio of the diethylenetriamine quality added and the thick tall oil waste residue of over dry is 0.18, mixes, at N
2be warming up to 150 DEG C under protective condition, reaction 3h, then forward in water distilling apparatus by solution, underpressure distillation is except removal xylene, and under room temperature, cooling obtains viscous liquid, is thick tall oil acid amides finished product.
(4) preparation of metal cutting emulsion, utilize the thick tall oil acid amides that above-mentioned steps (3) obtains, with the thick tall oil acid amides of mass percent 18.89%, 20.46% base oil, 4.79% boric acid, 0.50% dimethyl silicone oil, 10.0% trisodium phosphate, 1.54% polyoxyethylene glycol, 0.48% KF88, the OP-10 of 5.19%, the petroleum sodium sulfonate of 9.99% and surplus deionized water carry out Solution and emulsification about 1h at about 60 DEG C, obtain water-in-oil-type metal cutting emulsion.
Embodiment 6:
(1) neutralizing treatment of thick tall oil waste residue: first according to the pH value of liquid in waste residue, add that appropriate basic solution carries out stirring in room temperature, neutralization reaction, time is about 0.5h, in control and the pH value of waste liquid be about 6.0, leave standstill 3h, then remove lower floor's liquid, obtain treated thick tall oil waste residue;
(2) thick tal fibre oil separating: add dimethylbenzene as solvent in the thick tall oil waste residue obtained after above-mentioned (1) process, after abundant stirring and dissolving, filter cleaner, then leave standstill 2h, be separated removing water layer, obtain the xylene solution of thick tall oil;
(3) preparation of thick tall oil acid amides: in the thick tall oil xylene solution that above-mentioned (2) obtain, add the diethylenetriamine of requirement, the mass ratio of the diethylenetriamine quality added and the thick tall oil waste residue of over dry is 0.25, mixes, at N
2be warming up to 150 DEG C under protective condition, reaction 3h, then forward in water distilling apparatus by solution, underpressure distillation is except removal xylene, and under room temperature, cooling obtains viscous liquid, is thick tall oil acid amides finished product.
(4) preparation of metal cutting emulsion, utilize the thick tall oil acid amides that above-mentioned steps (3) obtains, with the thick tall oil acid amides of mass percent 18.89%, 20.46% base oil, 4.79% boric acid, 0.50% dimethyl silicone oil, 10.0% trisodium phosphate, 1.54% polyoxyethylene glycol, 0.48% KF88, the OP-10 of 5.19%, the petroleum sodium sulfonate of 9.99% and surplus deionized water carry out Solution and emulsification about 1h at about 60 DEG C, obtain water-in-oil-type metal cutting emulsion.
Embodiment 7:
(1) neutralizing treatment of thick tall oil waste residue: first according to the pH value of liquid in waste residue, add that appropriate basic solution carries out stirring in room temperature, neutralization reaction, time is about 0.5h, in control and the pH value of waste liquid be about 6.0, leave standstill 3h, then remove lower floor's liquid, obtain treated thick tall oil waste residue;
(2) thick tal fibre oil separating: add dimethylbenzene as solvent in the thick tall oil waste residue obtained after above-mentioned (1) process, after abundant stirring and dissolving, filter cleaner, then leave standstill 2h, be separated removing water layer, obtain the xylene solution of thick tall oil;
(3) preparation of thick tall oil acid amides: in the thick tall oil xylene solution that above-mentioned (2) obtain, add the diethylenetriamine of requirement, the mass ratio of the diethylenetriamine quality added and the thick tall oil waste residue of over dry is 0.18, mixes, at N
2be warming up to 150 DEG C under protective condition, reaction 3h, then forward in water distilling apparatus by solution, underpressure distillation is except removal xylene, and under room temperature, cooling obtains viscous liquid, is thick tall oil acid amides finished product.
(4) preparation of metal cutting emulsion, utilize the thick tall oil acid amides that above-mentioned steps (3) obtains, with the thick tall oil acid amides of mass percent 18.89%, 20.46% base oil, 4.79% boric acid, 0.50% dimethyl silicone oil, 10.0% trisodium phosphate, 1.54% polyoxyethylene glycol, 0.48% paraformaldehyde, the OP-10 of 5.19%, the petroleum sodium sulfonate of 9.99% and surplus deionized water carry out Solution and emulsification about 1h at about 60 DEG C, obtain water-in-oil-type metal cutting emulsion.
Embodiment 8:
(1) neutralizing treatment of thick tall oil waste residue: first according to the pH value of liquid in waste residue, add that appropriate basic solution carries out stirring in room temperature, neutralization reaction, time is about 0.5h, in control and the pH value of waste liquid be about 6.0, leave standstill 3h, then remove lower floor's liquid, obtain treated thick tall oil waste residue;
(2) thick tal fibre oil separating: add dimethylbenzene as solvent in the thick tall oil waste residue obtained after above-mentioned (1) process, after abundant stirring and dissolving, filter cleaner, then leave standstill 2h, be separated removing water layer, obtain the xylene solution of thick tall oil;
(3) preparation of thick tall oil acid amides: in the thick tall oil xylene solution that above-mentioned (2) obtain, add the diethylenetriamine of requirement, the mass ratio of the diethylenetriamine quality added and the thick tall oil waste residue of over dry is 0.18, mixes, at N
2be warming up to 150 DEG C under protective condition, reaction 3h, then forward in water distilling apparatus by solution, underpressure distillation is except removal xylene, and under room temperature, cooling obtains viscous liquid, is thick tall oil acid amides finished product.
(4) preparation of metal cutting emulsion, utilize the thick tall oil acid amides that above-mentioned steps (3) obtains, with the thick tall oil acid amides of mass percent 18.89%, 20.46% base oil, 4.79% boric acid, 0.50% dimethyl silicone oil, 10.0% trisodium phosphate, 1.54% polyoxyethylene glycol, 0.48% KF88, the OP-10 of 5.30%, the sodium laurylsulfonate of 9.80% and surplus deionized water carry out Solution and emulsification about 1h at about 60 DEG C, obtain water-in-oil-type metal cutting emulsion.
Embodiment 9:
(1) neutralizing treatment of thick tall oil waste residue: first according to the pH value of liquid in waste residue, add that appropriate basic solution carries out stirring in room temperature, neutralization reaction, time is about 0.5h, in control and the pH value of waste liquid be about 6.0, leave standstill 3h, then remove lower floor's liquid, obtain treated thick tall oil waste residue;
(2) thick tal fibre oil separating: add dimethylbenzene as solvent in the thick tall oil waste residue obtained after above-mentioned (1) process, after abundant stirring and dissolving, filter cleaner, then leave standstill 2h, be separated removing water layer, obtain the xylene solution of thick tall oil;
(3) preparation of thick tall oil acid amides: in the thick tall oil xylene solution that above-mentioned (2) obtain, add the diethylenetriamine of requirement, the mass ratio of the diethylenetriamine quality added and the thick tall oil waste residue of over dry is 0.18, mixes, at N
2be warming up to 150 DEG C under protective condition, reaction 3h, then forward in water distilling apparatus by solution, underpressure distillation is except removal xylene, and under room temperature, cooling obtains viscous liquid, is thick tall oil acid amides finished product.
(4) preparation of metal cutting emulsion, utilize the thick tall oil acid amides that above-mentioned steps (3) obtains, with the thick tall oil acid amides of mass percent 18.89%, 20.46% base oil, 4.79% boric acid, 0.50% dimethyl silicone oil, 10.0% trisodium phosphate, 1.54% polyoxyethylene glycol, 0.48% KF88, the OP-10 of 5.19%, the petroleum sodium sulfonate of 9.99% and surplus deionized water carry out Solution and emulsification about 2h at about 50 DEG C, obtain water-in-oil-type metal cutting emulsion.
Embodiment 10:
(1) neutralizing treatment of thick tall oil waste residue: first according to the pH value of liquid in waste residue, add that appropriate basic solution carries out stirring in room temperature, neutralization reaction, time is about 0.5h, in control and the pH value of waste liquid be about 6.0, leave standstill 3h, then remove lower floor's liquid, obtain treated thick tall oil waste residue;
(2) thick tal fibre oil separating: add dimethylbenzene as solvent in the thick tall oil waste residue obtained after above-mentioned (1) process, after abundant stirring and dissolving, filter cleaner, then leave standstill 2h, be separated removing water layer, obtain the xylene solution of thick tall oil;
(3) preparation of thick tall oil acid amides: in the thick tall oil xylene solution that above-mentioned (2) obtain, add the diethylenetriamine of requirement, the mass ratio of the diethylenetriamine quality added and the thick tall oil waste residue of over dry is 0.18, mixes, at N
2be warming up to 150 DEG C under protective condition, reaction 3h, then forward in water distilling apparatus by solution, underpressure distillation is except removal xylene, and under room temperature, cooling obtains viscous liquid, is thick tall oil acid amides finished product.
(4) preparation of metal cutting emulsion, utilize the thick tall oil acid amides that above-mentioned steps (3) obtains, with the thick tall oil acid amides of mass percent 18.89%, 20.46% base oil, 4.79% boric acid, 0.50% dimethyl silicone oil, 10.0% trisodium phosphate, 1.54% polyoxyethylene glycol, 0.48% KF88, the OP-10 of 5.19%, the petroleum sodium sulfonate of 9.99% and surplus deionized water carry out Solution and emulsification about 3h at about 40 DEG C, obtain water-in-oil-type metal cutting emulsion.
Metal cutting quality of the emulsion concentration prepared by the present invention is more than 70%, and stability reaches more than 6 months.
Screening formulation of the present invention is: the thick tall oil acid amides of mass percent 18.89%, the base oil of 20.46%, the boric acid of 4.79%, the dimethyl silicone oil of 0.50%, the trisodium phosphate of 10.0%, the polyoxyethylene glycol of 2.54%, the KF88 of 0.48%, the OP-10 of 5.19%, metal cutting emulsion prepared by the sodium laurylsulfonate of 9.99% and the deionized water of surplus, its use carries out package stability according to National Standard of the People's Republic of China GB/T6144-2010, pH measures, defoaming, transparency, the comparison test of the indexs such as corrodibility and monolithic rust-preventing characteristic, each metal cutting samples of latex carries out three parallel tests, result is as shown in table 1.
Table 1 metal cutting emulsion detected result
The metal cutting liquid emulsion process that the present invention is prepared for raw material with thick tall oil waste residue meets the corrosion resistance of national standard and the detection of rustless property, and its corrosion resistance reaches national B grade standard, and rustless property reaches national A grade standard.
Claims (10)
1. a method for the metal cutting emulsion utilizing thick tall oil waste residue to prepare, is characterized in that: adopt following steps:
(1) neutralizing treatment of thick tall oil waste residue: first according to the pH value of liquid in waste residue, add that appropriate basic solution carries out stirring, neutralization reaction, the liquid pH value controlling to produce is slightly acidic, leaves standstill, then remove lower floor's liquid, obtain thick tall oil waste residue after treatment;
(2) thick tal fibre oil separating: add organic solvent in the thick tall oil waste residue obtained after above-mentioned steps (1) process, after abundant stirring and dissolving, filter cleaner, then leave standstill, be separated removing water layer, obtain thick tall oil organic solution;
(3) preparation of thick tall oil acid amides: in the thick tall oil organic solution that above-mentioned steps (2) obtains, add the organic amine of requirement, mix, temperature reaction, underpressure distillation removing organic solvent again, cooling obtains viscous liquid, is thick tall oil acid amides finished product;
(4) the thick tall oil acid amides preparing metal obtained in above-mentioned steps (3) is utilized to cut emulsion.
2. method according to claim 1, it is characterized in that: source and the feature of the thick tall oil waste residue described in above-mentioned steps (1) are: contained grease and resin are converted into saponified in alkaline cooking process, be dissolved in black liquor, pass through enrichment process, saponifiedly float on black liquor liquid level, separated and collected is saponified, then wash with washings, remove saponified in part lignin, fiber and other impurity, and then carry out acidification reaction, be separated by standing sedimentation, upper strata is the thick tall oil that alkali lignin content is very low; Middle layer is then the mixolimnion of thick tall oil and alkali lignin, i.e. thick tall oil waste residue, and lower floor is spent acid solution; In the thick tall oil waste residue of gained, thick tall oil content is 40-70%, and alkali lignin content is 15-40%, and all the other are neutral unsaponifiables.
3. method according to claim 1, is characterized in that: step (1) neutralization reaction alkali lye used comprises: the solution of sodium hydroxide or sodium carbonate or ammoniacal liquor or trolamine.
4. method according to claim 1, is characterized in that: step (1) the neutralization reaction time is 0.5-1.0h, and the liquid pH value controlling to produce is 5.5-6.5, leaves standstill 2-4h, then removes lower floor's liquid, obtains thick tall oil waste residue after treatment.
5. method according to claim 1, is characterized in that: the organic solvent dissolving thick tall oil waste residue described in step (2) comprises benzene, toluene or dimethylbenzene.
6. method according to claim 1, it is characterized in that: in the thick tall oil organic solution in step (3), step (2) obtained, add the organic amine of requirement, the mass ratio of the organic amine quality added and the thick tall oil waste residue of over dry is 0.08-0.50, mixes.
7. method according to claim 1, is characterized in that: the organic amine described in step (3) comprises containing C
2~ C
6any one or several in the primary amine of carbochain, secondary amine, diamines, triamine, thanomin.
8. method according to claim 1, is characterized in that: at N in step (3)
2be warming up to 120-160 DEG C under protective condition, reaction 2-5h, then forward in water distilling apparatus by solution, underpressure distillation removing organic solvent, under room temperature, cooling obtains viscous liquid, is thick tall oil acid amides finished product.
9. method according to claim 1, it is characterized in that: step (4) utilizes in step (3) the thick tall oil acid amides obtained, with the base oil, stablizer, defoamer, sterilant, emulsifying agent, deionized water etc. of certain mass ratio 40 DEG C-70 DEG C carry out composite, dissolve and emulsification 1-3h, finally obtain metal cutting emulsion.
10. a metal cutting emulsion is prepared from by the method described in any one of claim 1-9.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6511946B1 (en) * | 1998-07-28 | 2003-01-28 | Fuchs Petrolub Ag | Water-miscible cooling lubricant concentrate |
| CN101704643A (en) * | 2009-11-06 | 2010-05-12 | 中南林业科技大学 | Method for producing concrete admixture by using coarse tall oil separated and refined slag |
| CN101768502A (en) * | 2010-01-29 | 2010-07-07 | 上海澳润科润滑剂有限公司 | Lubricating and cutting fluid |
| CN103805329A (en) * | 2014-03-03 | 2014-05-21 | 广州市联诺化工科技有限公司 | Special environment-friendly complete-synthesis cutting fluid for drilling stainless steel and preparation method thereof |
| CN104263245A (en) * | 2014-09-29 | 2015-01-07 | 中南林业科技大学 | Method for separating tall oil and alkali lignin from waste crude tall oil residues |
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2015
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6511946B1 (en) * | 1998-07-28 | 2003-01-28 | Fuchs Petrolub Ag | Water-miscible cooling lubricant concentrate |
| CN101704643A (en) * | 2009-11-06 | 2010-05-12 | 中南林业科技大学 | Method for producing concrete admixture by using coarse tall oil separated and refined slag |
| CN101768502A (en) * | 2010-01-29 | 2010-07-07 | 上海澳润科润滑剂有限公司 | Lubricating and cutting fluid |
| CN103805329A (en) * | 2014-03-03 | 2014-05-21 | 广州市联诺化工科技有限公司 | Special environment-friendly complete-synthesis cutting fluid for drilling stainless steel and preparation method thereof |
| CN104263245A (en) * | 2014-09-29 | 2015-01-07 | 中南林业科技大学 | Method for separating tall oil and alkali lignin from waste crude tall oil residues |
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