CN105385490B - A kind of metal cutting lotion and preparation method thereof prepared using thick tall oil waste residue - Google Patents

A kind of metal cutting lotion and preparation method thereof prepared using thick tall oil waste residue Download PDF

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CN105385490B
CN105385490B CN201510904181.5A CN201510904181A CN105385490B CN 105385490 B CN105385490 B CN 105385490B CN 201510904181 A CN201510904181 A CN 201510904181A CN 105385490 B CN105385490 B CN 105385490B
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thick
tall oil
waste residue
thick tall
oleamide
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CN105385490A (en
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蒋新元
万晓清
李秀清
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Central South University of Forestry and Technology
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Central South University of Forestry and Technology
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Abstract

The metal cutting lotion and preparation method thereof that the invention discloses a kind of to be prepared using thick tall oil waste residue, using following steps:(1) neutralisation treatment of thick tall oil waste residue;(2) separation of thick tall oil;(2) preparation of thick tal fibre oleamide;(3) thick tal fibre oleamide prepares metal cutting lotion with other ingredients.Tal fibre oleamide is made using the above method, is compounded and is emulsified in certain mass ratio with ingredients such as base oil, stabilizer, antifoaming agent, fungicide, emulsifier, deionized waters, stable metal cutting lotion can be obtained.The present invention passes through the detection of the corrosion resistance and rustless property that meet national standard using thick tall oil waste residue as metal cutting liquid emulsion prepared by raw material, and corrosion resistance reaches national B grades of standard, and rustless property reaches national A grades of standard.This method is not only easy to operate, moreover it is possible to which environmental protection reduces the discharge of waste, while improving enterprise's productive profit, reduces cost.

Description

A kind of metal cutting lotion and preparation method thereof prepared using thick tall oil waste residue
Technical field
The invention belongs to pine papermaking byproduct comprehensive utilization technical fields, are related to a kind of thick using pine pulping byproducts Metal cutting lotion and preparation method thereof prepared by tall oil waste residue.
Background technology
The pines such as south China masson pine are resourceful, are commonly used for the raw material of pulping and paper-making.China is in recent years with warp The development of Ji is rapidly developed by the pulping and paper-making industry of raw material of pine.In pine containing rosin, lignin, cellulose, The ingredients such as hemicellulose generate a large amount of by-product in pine alkaline cooking pulping process, as (also known as wood pulp is floating for tall oil Oil), sulfate turpentine, alkali lignin (black liquid) etc., it is comprehensive and effectively utilize by-product, can both economize on resources, protect Environment can also improve Business Economic Benefit and social environment.
Using pine as in the alkaline process of raw material or sulfate pulping digestion process, the grease in pine and resin component quilt Sodium salt that is saponification and forming aliphatic acid and resin acid is dissolved in black liquor, while neutral oil is also extracted and is dissolved in soap lye In, here it is sulfate soap (tall oils containing 50-55%wt), and lignin is then converted into alkali lignin and is dissolved in black liquor, as The sulfate soap of foam-like, aterrimus and foul smelling just floats on above black liquor, and concentrated black liquor is solid content 23%-32% When, it is put into big storage tank, hydrophilic resin acid soaps, fatty acid soaps, which are precipitated, at this time comes, and oil-soluble unsaponifiable matter is also extracted It takes out, floats to black liquor top and form Black liquor soap layer, saponified recycling storage is obtained sulfate soap.
The separation and Extraction of sulfate soap compound has settled process, aeration and centrifugal process etc..Settled process because of its production process not A large amount of foams occur, it is easy to operate, stable, efficient, it is not necessary to another oil (gas) filling device and be widely adopted.It is saponified to be stood in storagetank After separation and cleaning solution is sent to sink together, and the cleaning solution of strong basicity can remove effectively saponified middle 60-80%'s Lignin and about 50% fiber and impurity.It is washed in sink saponified to be supplied to acidification system again.It is saponified and sour After being reacted in reactor, the components such as thick tall oil, alkali lignin, fiber and gypsum are resolved into, while releasing H2S and CO2Gas Body, reactor upper layer are then the higher thick tall oil of purity, also referred to as tall oil, and lower layer is spent acid, waste water and solid precipitation Object etc., middle layer are the mixture containing ingredients such as tall oil, alkali lignin and neutral unsaponifiable matter, i.e., thick tall oil waste residue.According to Different pulping process and raw material, the content of thick tall oil and alkali lignin is different in the thick tall oil waste residue of gained, and general dryness is thick Thick tal fibre oil content is in 40%-70% in tall oil waste residue, and for alkali lignin content in 15%-40%, remaining is neutral not saponification Object.
The main component of thick tall oil is resin acid, aliphatic acid and neutrals, can be obtained after separation Starex acid, Floating oil fatty acid, tall oil pitch, distillation oil slick and hair oil, are one of the three big sources of rosin acid and aliphatic acid.If being refined Or tall oil is further isolated into the products such as rosin acid, aliphatic acid, then it can obtain more widely utilizing.
Starex acid:The structure of Starex acid is similar to gum rosin, and purposes is essentially identical with gum rosin.It is mainly used for The departments such as glue used in paper-making, soap, ink, paint, coating, resin.If being further processed into modified rosin or Starex spreading out Biology will be enlarged by its application field.
Floating oil fatty acid:Main component be oleic acid and linoleic acid, be widely used in plasticizer, liquid soap, synthetic detergent, Antifoaming agent etc..
Tall oil pitch is mainly made of high boiling neutrals, in addition to for departments such as adhesive, ink, paint, coating, Also extractable cupreol replaces cholest acid for manufacturing various anti arteriosclerosis drugs and vitamin etc..
The present invention is directed to the composition of thick tall oil waste residue, and neutralisation treatment, the system of tal fibre oleamide are taken to high oily waste residue It is standby, tal fibre oleamide detach, it is compound and emulsification the methods of prepare metal cutting lotion, by meeting the detection of national standard, Prepared cutting good emulsion stability, corrosion resistance reaches national B grades of standard, and rustless property reaches national A grades of standard, The needs of the metals such as iron, steel and copper anti-corrosion and antirust in cutting process can be met.
By above-mentioned utilization, the economic benefit of waste residue can be significantly improved, eliminates the pollution to environment, to promoting resource It recycles, realize that the sustainable development of society has great society and economic implications.
Invention content
The technical problem to be solved by the present invention is to the waste residues after being produced using the thick tall oil of by-product after pine slurrying For raw material, the metal cutting lotion for having higher economic value and the market demand is prepared, discharge and the environmental protection of waste are reduced, Enterprise's productive profit can be improved simultaneously, reduces cost.
In order to solve the above technical problem, the present invention provides the thick tall oil waste residue of utilization prepare the side of metal cutting lotion Method, using following steps:
(1) neutralisation treatment of thick tall oil waste residue:First according to the pH value of liquid in waste residue, suitable alkaline solution is added It is stirred, neutralization reaction, it is faintly acid to control generated liquid pH value, stands, then removes lower liquid, is obtained through place Thick tall oil waste residue after reason;
(2) separation of thick tall oil:It is added in the thick tall oil waste residue obtained after above-mentioned steps (1) processing organic molten Agent, after being sufficiently stirred dissolving, filtering and removing slag, then stand, it is separated off water layer, obtains thick tall oil organic solution;
(3) preparation of thick tal fibre oleamide:In the thick tall oil organic solution that above-mentioned steps (2) obtain, it is added and needs The organic amine of amount is uniformly mixed, temperature reaction, then is evaporated under reduced pressure removing organic solvent, and cooling obtains viscous liquid, as slightly Tal fibre oleamide finished product;
(4) the thick tal fibre oleamide preparing metal cutting lotion obtained in above-mentioned steps (3) is utilized.
The source of thick tall oil waste residue described in above-mentioned steps (1) and it is characterized in:Contained grease and resin are steamed in alkaline process It is converted into during boiling saponified, is dissolved in black liquor, it is saponified to float on black liquor liquid level by enrichment process, it separates and collects It is saponified, it is then washed with cleaning solution, then part lignin, fiber and other impurity during removal is saponified carry out again Acidification reaction is detached by standing sedimentation, and upper layer is the very low thick tall oil of alkali lignin content;Middle layer then be thick tall oil with The mixed layer of alkali lignin, i.e., thick tall oil waste residue, lower layer is acid pickle;Thick tal fibre oil content is in the thick tall oil waste residue of gained 40-70%, alkali lignin content are 15-40%, remaining is neutral unsaponifiable matter.
Lye includes used in step (1) neutralization reaction:The solution of sodium hydroxide or sodium carbonate or ammonium hydroxide or triethanolamine.
Step (1) the neutralization reaction time is 0.5-1.0h, and it is 5.5-6.5 to control generated liquid pH value, stands 2-4h, Then lower liquid is removed, thick tall oil waste residue after processing is obtained.
The organic solvent of the thick tall oil waste residue of dissolving described in step (2) includes benzene, toluene or dimethylbenzene.
In the thick tall oil organic solution for obtaining step (2) in step (3), the organic amine of requirement is added, is added The mass ratio of organic amine quality and the thick tall oil waste residue of over dry be 0.08-0.50, be uniformly mixed.
Organic amine described in step (3) includes containing C2~C6In the primary amine of carbochain, secondary amine, diamines, triamine, ethanol amine It is any one or several.
In N in step (3)2It is warming up to 120-160 DEG C under protective condition, reacts 2-5h, then solution is gone into distilling apparatus In, vacuum distillation removes organic solvent, and cooling at room temperature obtains viscous liquid, as thick tal fibre oleamide finished product.
Step (4) utilizes obtained thick tal fibre oleamide in step (3), with the base oil of certain mass ratio, stabilizer, Antifoaming agent, fungicide, emulsifier, deionized water are compounded, dissolved and are emulsified 1-3h at 40 DEG C -70 DEG C, finally obtain metal Cut lotion.
The present invention, which using thick tall oil waste residue prepares metal cutting lotion and solves, to be generated in thick tall oil producing process Waste residue due to its main component property is close and be difficult to efficiently separate and cause at present thick tall oil waste residue be not yet received effectively point The problem of from utilizing.Using the thick higher feature of tal fibre oil content in thick tall oil waste residue, by thick tall oil waste residue With processing, the detaching of thick tall oil, your thick oleamide the means such as preparation, compounding and emulsification, obtain corrosion resistance and reach state B grades of standards of family and rustless property reach national A grades of standard and the good metal cutting lotion of stability, can meet iron, steel, aluminium, conjunction The needs of the metal materials such as Jin Gang and copper anti-corrosion and antirust in cutting process, to realize tall oil in the waste residue It directly utilizes, the metal cutting lotion with higher economic value and the market demand is prepared, to improving the economic value of waste residue And enterprise profit, while influence of the waste residue to environment is reduced, there is positive meaning.
Specific implementation mode
With reference to specific embodiment, invention is further described in detail, and non-formation limitation of the present invention.
Embodiment 1:
(1) it is molten that suitable alkalinity is added first according to the pH value of liquid in waste residue in the neutralization and saponification of thick tall oil waste residue Liquid is stirred in room temperature, neutralization reaction, and the time is 0.5h or so, and the pH value that control neutralizes waste liquid is 6.0 or so, stands 3h, Then lower liquid is removed, treated thick tall oil waste residue is obtained;
(2) separation of thick tall oil:Toluene is added in the thick tall oil waste residue obtained after above-mentioned (1) is handled, fully stirs After mixing dissolving, filtering and removing slag, then 2h is stood, it is separated off water layer, obtains thick tall oil toluene solution;
(3) preparation of thick tal fibre oleamide:In the thick tall oil toluene solution that above-mentioned (2) obtain, requirement is added The mass ratio of ethylenediamine, the ethylenediamine quality being added and the thick tall oil waste residue of over dry is 0.10, is uniformly mixed, in N2Ceiling It is warming up to 150 DEG C under part, reacts 4h, then solution is gone in distilling apparatus, vacuum distillation removes toluene, and cooling at room temperature obtains Viscous liquid, as thick tal fibre oleamide finished product.
(4) preparation of metal cutting lotion:The thick tal fibre oleamide obtained using above-mentioned steps (3), with mass percent 18.89% thick tal fibre oleamide, 20.46% base oil, 4.79% boric acid, 0.50% dimethicone, 10.0% Sodium pyrophosphate, 1.54% polyethylene glycol, 0.48% Kathon, 5.19% OP-10,9.99% dodecyl sodium sulfate Solution and emulsification 1h or so are carried out at 60 DEG C or so with the deionized water of surplus, obtain water-in-oil type metal cutting lotion.
Embodiment 2:
(1) neutralisation treatment of thick tall oil waste residue:First according to the pH value of liquid in waste residue, suitable alkaline solution is added It is stirred in room temperature, neutralization reaction, the time is 0.5h or so, and the pH value that control neutralizes waste liquid is 6.0 or so, stands 3h, so After remove lower liquid, obtain processed thick tall oil waste residue;
(2) separation of thick tall oil:Dimethylbenzene is added in the thick tall oil waste residue obtained after above-mentioned (1) is handled as molten Agent, after being sufficiently stirred dissolving, filtering and removing slag, then 2h is stood, it is separated off water layer, obtains the xylene solution of thick tall oil;
(3) preparation of thick tal fibre oleamide:In the thick tall oil xylene solution that above-mentioned (2) obtain, requirement is added Ethylenediamine, the mass ratio of the ethylenediamine quality being added and the thick tall oil waste residue of over dry is 0.10, is uniformly mixed, in N2Protection Under the conditions of be warming up to 150 DEG C, react 4h, then solution is gone in distilling apparatus, vacuum distillation removes removal xylene, cools down at room temperature Viscous liquid is obtained, as thick tal fibre oleamide finished product.
(4) preparation of metal cutting lotion, the thick tal fibre oleamide obtained using above-mentioned steps (3), with mass percent 18.89% thick tal fibre oleamide, 20.46% base oil, 4.79% boric acid, 0.50% dimethicone, 10.0% Sodium pyrophosphate, 1.54% polyethylene glycol, 0.48% Kathon, 5.19% OP-10,9.99% petroleum sodium sulfonate and remaining The deionized water of amount carries out Solution and emulsification 1h or so at 60 DEG C or so, obtains water-in-oil type metal cutting lotion.
Embodiment 3:
(1) neutralisation treatment of thick tall oil waste residue:First according to the pH value of liquid in waste residue, suitable alkaline solution is added It is stirred in room temperature, neutralization reaction, the time is 0.5h or so, and the pH value that control neutralizes waste liquid is 6.0 or so, stands 3h, so After remove lower liquid, obtain processed thick tall oil waste residue;
(2) separation of thick tall oil:Dimethylbenzene is added in the thick tall oil waste residue obtained after above-mentioned (1) is handled as molten Agent, after being sufficiently stirred dissolving, filtering and removing slag, then 2h is stood, it is separated off water layer, obtains the xylene solution of thick tall oil;
(3) preparation of thick tal fibre oleamide:In the thick tall oil xylene solution that above-mentioned (2) obtain, requirement is added Diethylenetriamine, the mass ratio of the diethylenetriamine quality being added and the thick tall oil waste residue of over dry is 0.18, is uniformly mixed, In N2It is warming up to 150 DEG C under protective condition, reacts 3h, then solution is gone in distilling apparatus, vacuum distillation removes removal xylene, room The lower cooling of temperature obtains viscous liquid, as thick tal fibre oleamide finished product.
(4) preparation of metal cutting lotion, the thick tal fibre oleamide obtained using above-mentioned steps (3), with mass percent 18.89% thick tal fibre oleamide, 20.46% base oil, 4.79% boric acid, 0.50% dimethicone, 10.0% Sodium pyrophosphate, 1.54% polyethylene glycol, 0.48% Kathon, 5.19% OP-10,9.99% petroleum sodium sulfonate and remaining The deionized water of amount carries out Solution and emulsification 1h or so at 60 DEG C or so, obtains water-in-oil type metal cutting lotion.
Embodiment 4:
(1) neutralisation treatment of thick tall oil waste residue:First according to the pH value of liquid in waste residue, suitable alkaline solution is added It being stirred in room temperature, neutralization reaction, the time is 1.0h or so, and the pH value that control neutralizes waste liquid is 6.0 or so, stands 2-4h, Then lower liquid is removed, processed thick tall oil waste residue is obtained;
(2) separation of thick tall oil:Dimethylbenzene is added in the thick tall oil waste residue obtained after above-mentioned (1) is handled as molten Agent, after being sufficiently stirred dissolving, filtering and removing slag, then 1-2h is stood, it is separated off water layer, obtains the xylene solution of thick tall oil;
(3) preparation of thick tal fibre oleamide:In the thick tall oil xylene solution that above-mentioned (2) obtain, requirement is added Diethanol amine, the mass ratio of the diethanol amine quality being added and the thick tall oil waste residue of over dry is 0.19, is uniformly mixed, in N2 It is warming up to 160 DEG C under protective condition, reacts 5h, then solution is gone in distilling apparatus, vacuum distillation removes removal xylene, at room temperature Cooling obtains viscous liquid, as thick tal fibre oleamide finished product.
(4) preparation of metal cutting lotion, the thick tal fibre oleamide obtained using above-mentioned steps (3), with mass percent 18.89% thick tal fibre oleamide, 20.46% base oil, 4.79% boric acid, 0.50% dimethicone, 10.0% Sodium pyrophosphate, 1.54% polyethylene glycol, 0.48% Kathon, 5.19% OP-10,9.99% petroleum sodium sulfonate and remaining The deionized water of amount carries out Solution and emulsification 1h or so at 60 DEG C or so, obtains water-in-oil type metal cutting lotion.
Embodiment 5:
(1) neutralisation treatment of thick tall oil waste residue:First according to the pH value of liquid in waste residue, suitable alkaline solution is added It is stirred in room temperature, neutralization reaction, the time is 0.5h or so, and the pH value that control neutralizes waste liquid is 6.0 or so, stands 3h, so After remove lower liquid, obtain processed thick tall oil waste residue;
(2) separation of thick tall oil:Dimethylbenzene is added in the thick tall oil waste residue obtained after above-mentioned (1) is handled as molten Agent, after being sufficiently stirred dissolving, filtering and removing slag, then 2h is stood, it is separated off water layer, obtains thick tall oil xylene solution;
(3) preparation of thick tal fibre oleamide:In the thick tall oil xylene solution that above-mentioned (2) obtain, requirement is added Diethylenetriamine, the mass ratio of the diethylenetriamine quality being added and the thick tall oil waste residue of over dry is 0.18, is uniformly mixed, In N2It is warming up to 150 DEG C under protective condition, reacts 3h, then solution is gone in distilling apparatus, vacuum distillation removes removal xylene, room The lower cooling of temperature obtains viscous liquid, as thick tal fibre oleamide finished product.
(4) preparation of metal cutting lotion, the thick tal fibre oleamide obtained using above-mentioned steps (3), with mass percent 18.89% thick tal fibre oleamide, 20.46% base oil, 4.79% boric acid, 0.50% dimethicone, 10.0% Sodium pyrophosphate, 1.54% polyethylene glycol, 0.48% Kathon, 5.19% OP-10,9.99% petroleum sodium sulfonate and remaining The deionized water of amount carries out Solution and emulsification 1h or so at 60 DEG C or so, obtains water-in-oil type metal cutting lotion.
Embodiment 6:
(1) neutralisation treatment of thick tall oil waste residue:First according to the pH value of liquid in waste residue, suitable alkaline solution is added It is stirred in room temperature, neutralization reaction, the time is 0.5h or so, and the pH value that control neutralizes waste liquid is 6.0 or so, stands 3h, so After remove lower liquid, obtain processed thick tall oil waste residue;
(2) separation of thick tall oil:Dimethylbenzene is added in the thick tall oil waste residue obtained after above-mentioned (1) is handled as molten Agent, after being sufficiently stirred dissolving, filtering and removing slag, then 2h is stood, it is separated off water layer, obtains the xylene solution of thick tall oil;
(3) preparation of thick tal fibre oleamide:In the thick tall oil xylene solution that above-mentioned (2) obtain, requirement is added Diethylenetriamine, the mass ratio of the diethylenetriamine quality being added and the thick tall oil waste residue of over dry is 0.25, is uniformly mixed, In N2It is warming up to 150 DEG C under protective condition, reacts 3h, then solution is gone in distilling apparatus, vacuum distillation removes removal xylene, room The lower cooling of temperature obtains viscous liquid, as thick tal fibre oleamide finished product.
(4) preparation of metal cutting lotion, the thick tal fibre oleamide obtained using above-mentioned steps (3), with mass percent 18.89% thick tal fibre oleamide, 20.46% base oil, 4.79% boric acid, 0.50% dimethicone, 10.0% Sodium pyrophosphate, 1.54% polyethylene glycol, 0.48% Kathon, 5.19% OP-10,9.99% petroleum sodium sulfonate and remaining The deionized water of amount carries out Solution and emulsification 1h or so at 60 DEG C or so, obtains water-in-oil type metal cutting lotion.
Embodiment 7:
(1) neutralisation treatment of thick tall oil waste residue:First according to the pH value of liquid in waste residue, suitable alkaline solution is added It is stirred in room temperature, neutralization reaction, the time is 0.5h or so, and the pH value that control neutralizes waste liquid is 6.0 or so, stands 3h, so After remove lower liquid, obtain processed thick tall oil waste residue;
(2) separation of thick tall oil:Dimethylbenzene is added in the thick tall oil waste residue obtained after above-mentioned (1) is handled as molten Agent, after being sufficiently stirred dissolving, filtering and removing slag, then 2h is stood, it is separated off water layer, obtains the xylene solution of thick tall oil;
(3) preparation of thick tal fibre oleamide:In the thick tall oil xylene solution that above-mentioned (2) obtain, requirement is added Diethylenetriamine, the mass ratio of the diethylenetriamine quality being added and the thick tall oil waste residue of over dry is 0.18, is uniformly mixed, In N2It is warming up to 150 DEG C under protective condition, reacts 3h, then solution is gone in distilling apparatus, vacuum distillation removes removal xylene, room The lower cooling of temperature obtains viscous liquid, as thick tal fibre oleamide finished product.
(4) preparation of metal cutting lotion, the thick tal fibre oleamide obtained using above-mentioned steps (3), with mass percent 18.89% thick tal fibre oleamide, 20.46% base oil, 4.79% boric acid, 0.50% dimethicone, 10.0% Sodium pyrophosphate, 1.54% polyethylene glycol, 0.48% paraformaldehyde, 5.19% OP-10,9.99% petroleum sodium sulfonate Solution and emulsification 1h or so are carried out at 60 DEG C or so with the deionized water of surplus, obtain water-in-oil type metal cutting lotion.
Embodiment 8:
(1) neutralisation treatment of thick tall oil waste residue:First according to the pH value of liquid in waste residue, suitable alkaline solution is added It is stirred in room temperature, neutralization reaction, the time is 0.5h or so, and the pH value that control neutralizes waste liquid is 6.0 or so, stands 3h, so After remove lower liquid, obtain processed thick tall oil waste residue;
(2) separation of thick tall oil:Dimethylbenzene is added in the thick tall oil waste residue obtained after above-mentioned (1) is handled as molten Agent, after being sufficiently stirred dissolving, filtering and removing slag, then 2h is stood, it is separated off water layer, obtains the xylene solution of thick tall oil;
(3) preparation of thick tal fibre oleamide:In the thick tall oil xylene solution that above-mentioned (2) obtain, requirement is added Diethylenetriamine, the mass ratio of the diethylenetriamine quality being added and the thick tall oil waste residue of over dry is 0.18, is uniformly mixed, In N2It is warming up to 150 DEG C under protective condition, reacts 3h, then solution is gone in distilling apparatus, vacuum distillation removes removal xylene, room The lower cooling of temperature obtains viscous liquid, as thick tal fibre oleamide finished product.
(4) preparation of metal cutting lotion, the thick tal fibre oleamide obtained using above-mentioned steps (3), with mass percent 18.89% thick tal fibre oleamide, 20.46% base oil, 4.79% boric acid, 0.50% dimethicone, 10.0% Sodium pyrophosphate, 1.54% polyethylene glycol, 0.48% Kathon, 5.30% OP-10,9.80% dodecyl sodium sulfate Solution and emulsification 1h or so are carried out at 60 DEG C or so with the deionized water of surplus, obtain water-in-oil type metal cutting lotion.
Embodiment 9:
(1) neutralisation treatment of thick tall oil waste residue:First according to the pH value of liquid in waste residue, suitable alkaline solution is added It is stirred in room temperature, neutralization reaction, the time is 0.5h or so, and the pH value that control neutralizes waste liquid is 6.0 or so, stands 3h, so After remove lower liquid, obtain processed thick tall oil waste residue;
(2) separation of thick tall oil:Dimethylbenzene is added in the thick tall oil waste residue obtained after above-mentioned (1) is handled as molten Agent, after being sufficiently stirred dissolving, filtering and removing slag, then 2h is stood, it is separated off water layer, obtains the xylene solution of thick tall oil;
(3) preparation of thick tal fibre oleamide:In the thick tall oil xylene solution that above-mentioned (2) obtain, requirement is added Diethylenetriamine, the mass ratio of the diethylenetriamine quality being added and the thick tall oil waste residue of over dry is 0.18, is uniformly mixed, In N2It is warming up to 150 DEG C under protective condition, reacts 3h, then solution is gone in distilling apparatus, vacuum distillation removes removal xylene, room The lower cooling of temperature obtains viscous liquid, as thick tal fibre oleamide finished product.
(4) preparation of metal cutting lotion, the thick tal fibre oleamide obtained using above-mentioned steps (3), with mass percent 18.89% thick tal fibre oleamide, 20.46% base oil, 4.79% boric acid, 0.50% dimethicone, 10.0% Sodium pyrophosphate, 1.54% polyethylene glycol, 0.48% Kathon, 5.19% OP-10,9.99% petroleum sodium sulfonate and remaining The deionized water of amount carries out Solution and emulsification 2h or so at 50 DEG C or so, obtains water-in-oil type metal cutting lotion.
Embodiment 10:
(1) neutralisation treatment of thick tall oil waste residue:First according to the pH value of liquid in waste residue, suitable alkaline solution is added It is stirred in room temperature, neutralization reaction, the time is 0.5h or so, and the pH value that control neutralizes waste liquid is 6.0 or so, stands 3h, so After remove lower liquid, obtain processed thick tall oil waste residue;
(2) separation of thick tall oil:Dimethylbenzene is added in the thick tall oil waste residue obtained after above-mentioned (1) is handled as molten Agent, after being sufficiently stirred dissolving, filtering and removing slag, then 2h is stood, it is separated off water layer, obtains the xylene solution of thick tall oil;
(3) preparation of thick tal fibre oleamide:In the thick tall oil xylene solution that above-mentioned (2) obtain, requirement is added Diethylenetriamine, the mass ratio of the diethylenetriamine quality being added and the thick tall oil waste residue of over dry is 0.18, is uniformly mixed, In N2It is warming up to 150 DEG C under protective condition, reacts 3h, then solution is gone in distilling apparatus, vacuum distillation removes removal xylene, room The lower cooling of temperature obtains viscous liquid, as thick tal fibre oleamide finished product.
(4) preparation of metal cutting lotion, the thick tal fibre oleamide obtained using above-mentioned steps (3), with mass percent 18.89% thick tal fibre oleamide, 20.46% base oil, 4.79% boric acid, 0.50% dimethicone, 10.0% Sodium pyrophosphate, 1.54% polyethylene glycol, 0.48% Kathon, 5.19% OP-10,9.99% petroleum sodium sulfonate and remaining The deionized water of amount carries out Solution and emulsification 3h or so at 40 DEG C or so, obtains water-in-oil type metal cutting lotion.
70% or more, stability reaches 6 months or more metal cutting quality of the emulsion concentration prepared by the present invention.
Optimization formula of the present invention is:The thick tal fibre oleamide of mass percent 18.89%, 20.46% base oil, 4.79% boric acid, 0.50% dimethicone, 10.0% sodium pyrophosphate, 2.54% polyethylene glycol, 0.48% it is triumphant Metal cutting lotion prepared by the deionized water of pine, 5.19% OP-10,9.99% dodecyl sodium sulfate and surplus, Bin stability, pH measurements, defoaming, saturating is carried out using according to National Standard of the People's Republic of China GB/T 6144-2010 The comparison test of the indexs such as lightness, corrosivity and monolithic rust-preventing characteristic, each metal cutting samples of latex carry out parallel test three times, The results are shown in Table 1.
1 metal cutting lotion testing result of table
The present invention passes through the anti-corruption for meeting national standard using thick tall oil waste residue as metal cutting liquid emulsion prepared by raw material Corrosion can reach national B grades of standard with the detection of rustless property, corrosion resistance, and rustless property reaches national A grades of standard.

Claims (8)

1. a kind of method of the metal cutting lotion prepared using thick tall oil waste residue, it is characterized in that:Using following steps:
(1) neutralisation treatment of thick tall oil waste residue:First according to the pH value of liquid in waste residue, suitable alkaline solution is added and carries out Stirring, neutralization reaction, it is faintly acid to control generated liquid pH value, stands, then removes lower liquid, obtain after processing Thick tall oil waste residue;
(2) separation of thick tall oil:Organic solvent is added in the thick tall oil waste residue obtained after above-mentioned steps (1) processing, fills After dividing stirring and dissolving, filtering and removing slag, then stand, it is separated off water layer, obtains thick tall oil organic solution;
(3) preparation of thick tal fibre oleamide:In the thick tall oil organic solution that above-mentioned steps (2) obtain, requirement is added Organic amine is uniformly mixed, temperature reaction, then is evaporated under reduced pressure removing organic solvent, and cooling obtains viscous liquid, as thick tal fibre Oleamide finished product;
(4) the thick tal fibre oleamide preparing metal cutting lotion obtained in above-mentioned steps (3) is utilized;
In the thick tall oil organic solution for step (2) being obtained in step (3), be added the organic amine of requirement, what is be added has The mass ratio of machine amine quality and the thick tall oil waste residue of over dry is 0.08-0.50, is uniformly mixed;
Organic amine described in step (3) includes containing C2~C6Appointing in the primary amine of carbochain, secondary amine, diamines, triamine, ethanol amine It is one or more of.
2. according to the method described in claim 1, it is characterized in that:The source of thick tall oil waste residue described in above-mentioned steps (1) Be characterized in:Contained grease and resin are converted into saponified during alkaline cooking, are dissolved in black liquor, pass through and concentrate work Sequence, it is saponified to float on black liquor liquid level, it separates and collects saponified, is then washed with cleaning solution, the portion during removal is saponified Point lignin, fiber and other impurity, then carry out acidification reaction, are detached by standing sedimentation again, upper layer be alkali lignin content very Low thick tall oil;Middle layer is then the mixed layer of thick tall oil and alkali lignin, i.e., thick tall oil waste residue, lower layer is acid pickle; Thick tal fibre oil content is 40-70% in the thick tall oil waste residue of gained, and alkali lignin content is 15-40%, remaining is neutral not saponification Object.
3. according to the method described in claim 1, it is characterized in that:Lye includes used in step (1) neutralization reaction:Sodium hydroxide or The solution of sodium carbonate or ammonium hydroxide or triethanolamine.
4. according to the method described in claim 1, it is characterized in that:Step (1) the neutralization reaction time is 0.5-1.0h, and control is produced Raw liquid pH value is 5.5-6.5, stands 2-4h, then removes lower liquid, obtain thick tall oil waste residue after processing.
5. according to the method described in claim 1, it is characterized in that:The organic molten of thick tall oil waste residue is dissolved described in step (2) Agent includes benzene, toluene or dimethylbenzene.
6. according to the method described in claim 1, it is characterized in that:In N in step (3)2It is warming up to 120-160 DEG C under protective condition, 2-5h is reacted, then solution is gone in distilling apparatus, vacuum distillation removes organic solvent, and cooling at room temperature obtains thick liquid Body, as thick tal fibre oleamide finished product.
7. according to the method described in claim 1, it is characterized in that:Step (4) utilizes the thick tal fibre oleoyl obtained in step (3) Amine is carried out with the base oil of certain mass ratio, stabilizer, antifoaming agent, fungicide, emulsifier, deionized water at 40 DEG C -70 DEG C Compounding, dissolving and emulsification 1-3h, finally obtain metal cutting lotion.
8. a kind of metal cutting lotion is prepared by claim 1-7 any one of them methods.
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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

Patent Citations (5)

* Cited by examiner, † Cited by third party
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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