CN1974730A - Process of producing oxygenated paraffin soap - Google Patents
Process of producing oxygenated paraffin soap Download PDFInfo
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- CN1974730A CN1974730A CN 200610134693 CN200610134693A CN1974730A CN 1974730 A CN1974730 A CN 1974730A CN 200610134693 CN200610134693 CN 200610134693 CN 200610134693 A CN200610134693 A CN 200610134693A CN 1974730 A CN1974730 A CN 1974730A
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Abstract
The process of producing oxygenated paraffin soap includes the steps of: preparing material, preparing oxidized paraffin, saponification, refining and packing. Reclaimed wax is extracted from the un-saponified matter separated from the soap liquid after saponification of oxidized paraffin, and mixed to the material paraffin, with the ratio between the reclaimed wax and the material paraffin being 2-4 to 6-8. The oxygenated paraffin soap has effective component content over 60 %, greatly shortened technological process, and high product yield.
Description
Technical field
The present invention relates to a kind of Chemicals, particularly relate to a kind of process of producing oxygenated paraffin soap, is the improvement to existing process of producing oxygenated paraffin soap, belongs to the technology of preparing of Chemicals.
Background technology
Oxidized paraffin wax soap is as a kind of flotation reagent, be mainly used in the flotation in burning ore deposit, the weak point that its existing production method exists is: adopt the low air quantity oxidation of low temperature, main effective constituent is low in the resultant, reaction is slow, the time is long, both increased production cost, and influenced product again and mainly contain effective component content.And the oil-soluble acid that oxidizing reaction generates do not participate in saponification, can not get recycling, in the storage just in case leakage can cause environmental pollution.
Summary of the invention
The objective of the invention is to overcome the prior art above shortcomings, improve at existing process of producing oxygenated paraffin soap, provide a kind of new process of producing oxygenated paraffin soap, main effective constituent can be up to more than 60% in the oxidation resultant among the present invention, the comparable existing technology of oxidization time shortens 10 hours, and the oil-soluble acid that oxidizing reaction generates is participated in saponification, has both increased product yield, promote that again saponification reaction speeds up, the soap lye layering is fast and obvious.
The technical scheme that the present invention provides is: this process of producing oxygenated paraffin soap is characterized in being made up of following steps:
1. get the raw materials ready: a certain amount of paraffin is squeezed in the preheating can, impurities removal, Fen Shui, dewater and be warming up to 120 ℃ after the insulation standby, additive sylvite and manganese salt drop in the dissolving vessel by 0.3～0.8 ‰ by charging capacity 1.5～2 ‰, soda ash, it is standby to add water-solubleization back, get the caustic soda of inventory about 50%, make behind the alkaline solution of concentration 25-30% standby;
2. the preparation of oxidized petroleum waves: the material that preheating in the preheating can is good is squeezed in the oxidizing tower, simultaneously by 40 cubic metres/tons per hour air quantity air feed in oxidizing tower, heat supply, catalyst solution is squeezed in the tower, when temperature of charge in the tower reaches 160 ± 2 ℃, begin to cause, kept 0.5 hour, wind supply quantity is brought up to 50 cubic metres/tons per hour, be cooled to 150 ± 2 ℃ and begin to excite, after two hours, material is cooled to 120-130 ℃ in the tower, the beginning oxidation, simultaneously wind supply quantity is increased to 60 cubic metres/tons per hour, and is temperature-resistant, and 80 cubic metres/tons per hour after 12 hours is brought up to air quantity in oxidation, temperature-resistant, begin to detect acid number after exciting end, when oxidizing tower material acid number reached 80-85mgKOH/g, oxidation finished, after oxidation finishes, material stops heat supply and is cooled to 120 ℃ in the tower, simultaneously wind supply quantity is reduced to 40 cubic metres/tons per hour, begins tower, material in the oxidizing tower is squeezed in the saponification jar that tankage 30-40%75 ℃ hot water is housed, will be reacted the oil-soluble acid that generates simultaneously and evenly squeeze into the saponification jar;
3. saponification:
(1). washing: the oxidized petroleum waves temperature that will squeeze into the saponification jar is adjusted to about 85 ℃, with steam or air, transfer to material and seethe state, when temperature of charge is lower than 85 ℃ in the saponification jar, stir with open steam, when being higher than 85 ℃, uses temperature of charge pneumatic blending instead, stirred at least 40 minutes, stirring stops the back and be incubated sedimentation under 85-90 ℃ of condition, sedimentation was discharged waste water and middle layer from the saponification pot bottom after 30 minutes, till detection washing rear oxidation cerinic acid value was slightly acidic to the waste water pH value, defective will the repetition washed;
(2). saponification: the oxidized petroleum waves qualified to washing in the saponification jar, with being steam heated to 95-100 ℃, the water that adds inventory about 35% simultaneously under material boiling situation, adds the alkaline solution of getting ready in the oxidized petroleum waves, adding alkali number calculates by oxidized petroleum waves alkali charge=acid number per ton * 1.8 * 0.71 * 1.03 (excess base) ÷ concentration ÷ 1000, filled up the alkali after saponification 1 hour, the recirculation saponification is more than 1 hour, and saponification finishes back check pH value about 13, saponification is finished, otherwise continues alkaline saponification;
(3). separate: after saponification finished, material insulation sedimentation was at least 3 hours in the saponification jar, and soap lye is squeezed into the soap lye storage tank, surpassed rest time to change next procedure again over to after 24 hours;
4. refining: soap lye qualified in the storage tank is squeezed into tube furnace through pressure pump, adjust inlet amount and measure with fire, squeeze into during when material moisture and to be the oxidized paraffin wax soap work in-process in the treatment tank in 30% left and right sides, after check, adjust free alkali content, moisture, make it reach standard-required, material is qualified after testing in the treatment tank is finished product, and squeezes into the finished product jar and carry out metering packing.
Purpose to better implement the present invention, in the oxidized petroleum waves saponification process of described step 3, remainder after soap lye separates is a unsaponifiables, this unsaponifiables adds acid treatment under agitation condition, temperature of charge keeps 80 ± 5 ℃, stirred at least 40 minutes, adding sour terminal point, to be controlled at the material pH value be 3-2, and static at least 1 hour of material separates waste liquid down from jar, remaining yellow substance is for reclaiming wax, in the saponification jar, add the warm water washing, discharge waste water and interstitial impurity at least after static 1 hour, after the detection acid number is qualified reclaiming wax, it is standby to squeeze into recovery wax storage tank, detects defective repetition of acid number and washes.
Purpose to better implement the present invention, the paraffin in the described step 1 can replace with partially recycled wax, wherein paraffin: reclaim wax in 6～8: 2～4 ratio is better.
Purpose to better implement the present invention, the adjustment of the free alkali in the described step 4 for transferring to 0.8% with caustic soda soln earlier, adds inventory 1% soda ash again.
The raw material that the present invention uses, all same as the prior art as soap wax, catalyzer, caustic soda, soda ash, can purchase from the market, reclaim wax for the one-level unsaponifiables that reclaims among the present invention etc., impurity elimination, dehydration, wherein soap wax: fusing point 30-50 ℃, oleaginousness 8-15%, appearance white or yellow, catalyzer: manganese salt and sylvite, technical grade, caustic soda: technical grade, content is more than 96%, soda ash: technical grade.
The main production equipments that the present invention uses: oxidizing tower, gas blower, air compressor machine, preheating can, catalyst dissolution jar, alkali solving can, alkali test tank, saponification jar, tube furnace, molten soap jar, treatment tank, finished product jar, common equipment in the same industry belongs to prior art.
The main quality index such as the following table of the product oxidized paraffin wax soap that the present invention provides are listed:
| Project | Quality index | Test method |
| Outward appearance | The Vandyke brown paste | Range estimation |
| Fatty acid content % 〉= | 50 | Q116-2002 |
| Unsaponifiables≤ | 15 | Q116-2002 |
| Free alkali NaOH≤ | 1.0 | GB/T260-77 |
| Moisture %≤ | 30 | SH/T0329 |
Compared with prior art, the invention has the beneficial effects as follows: main effective constituent can be up to more than 60% in the oxidation resultant among the present invention, the comparable existing technology of oxidization time shortens 10 hours, the oil-soluble acid that oxidizing reaction generates is participated in saponification, both increased product yield, promote that again saponification reaction speeds up, the soap lye layering is fast and obvious.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further.
Embodiment 1
At first paraffin, recovery wax are squeezed in the preheating can in 6: 4 ratios, impurities removal, Fen Shui, dewater and to be warming up to 120 ℃ of insulations standby, sylvite and manganese salt are by charging capacity 1.6 ‰, soda ash drops in the dissolving vessel by 0.4 ‰, add proper amount of clear water and the heating dissolve standby, get the caustic soda of inventory 50%, the alkaline solution of making concentration 25% is standby;
Again that preheating in the preheating can is good material is squeezed in the oxidizing tower, open gas blower simultaneously, by 40 cubic metres/tons per hour air quantity air feed in oxidizing tower, and capacity is to the heat supply of tower internal heating system, catalyst solution is squeezed in the tower, when temperature of charge in the tower reaches 160 ± 2 ℃, begin to cause, kept 0.5 hour, wind supply quantity is brought up to 50 cubic metres/tons per hour, being cooled to 150 ± 2 ℃ begins to excite, kept with this understanding two hours, the interior material of tower is cooled to 120-130 ℃ after two hours, the beginning oxidation, simultaneously wind supply quantity is increased to 60 cubic metres/tons per hour, and temperature remains unchanged, and 80 cubic metres/tons per hour after 12 hours is brought up to air quantity in oxidation, temperature remains unchanged, after exciting end, begin to detect acid number, detected the once oxidation acid number in per 4 hours, every two hours detected the once oxidation acid number in 16 hours later on, when oxidizing tower material acid number reaches 80-85mgKOH/g, oxidation finishes, and after oxidation finished, material stopped heat supply and is cooled to 120 ℃ in the tower, simultaneously wind supply quantity is reduced to 40 cubic metres/tons per hour, begin tower, material in the oxidizing tower is squeezed in the saponification jar that 30-40%75 ℃ of hot water is housed, will react the oil-soluble acid that generates simultaneously and evenly squeeze into the saponification jar;
Wash then, saponification.The oxidized petroleum waves temperature that to squeeze into the saponification jar earlier is adjusted to about 85 ℃, with steam directly to the material type of heating steam supply that blows slowly, and transfer to material and seethe state, when temperature of charge is lower than 85 ℃ in the saponification jar, stir with open steam, when being higher than 85 ℃, uses temperature of charge pneumatic blending instead, stirred 40 minutes, stop to stir, under 85-90 ℃ of condition, be incubated sedimentation, after the sedimentation 30 minutes, discharge waste water and middle layer from the saponification pot bottom, repeat to be washed to the waste water pH value and be till the slightly acidic, detect washing rear oxidation cerinic acid value; Qualified to washing in the saponification jar again oxidized petroleum waves, be heated to 95-100 ℃ with open steam, the clear water that adds inventory about 35% simultaneously, under material boiling situation, slowly add the alkaline solution of getting ready in the oxidized petroleum waves, adding alkali number is calculated as follows: oxidized petroleum waves alkali charge=acid number per ton * 1.8 * 0.71 * 1.03 (excess base) ÷ concentration ÷ 1000, after filling up alkali by calculated amount, saponification 1 hour, the recirculation saponification is more than 1 hour, total saponification time was not less than two hours, saponification finishes the back with phenolphthalein indicator and the check of PH test paper, makes the phenolphthalein pinkiness, pH value about 13, saponification is finished, otherwise continues alkaline saponification; After saponification finished, material insulation sedimentation was 3 hours in the saponification jar, squeezes into the soap lye storage tank by saponification bottom valve goalkeeper soap lye, will beat slowly when buying soap lye, beat while observing, the later stage will stop to beat, prevent that unsaponifiables from sneaking into, surpass 24 hours rest time and can change next procedure over to;
At last soap lye qualified in the storage tank is squeezed into tube furnace through pressure pump, adjust inlet amount and measure with fire, make the tube furnace temperature out reach 120 ℃, material moisture is about 30%, squeeze into and be the oxidized paraffin wax soap work in-process in the treatment tank, after check, adjust free alkali content, moisture, make its requirement that touches the mark, the adjustment of free alkali will transfer to 0.8% with caustic soda soln, adds inventory 1% soda ash again, the qualified after testing finished product that is of material in the treatment tank, through refining qualified oxidized paraffin wax soap, squeeze into the finished product jar, by the accurate metering packing of weight of 40 kilograms in every case, packing material adopts carton, in add plastics for lining, and indicate title, date, order of classes or grades at school, lot number, gross weight, net weight etc.
The main quality index such as the following table of oxidized paraffin wax soap are listed:
| Project | Quality index | Test method |
| Outward appearance | The Vandyke brown paste | Range estimation |
| Fatty acid content % 〉= | 50 | Q116-2002 |
| Unsaponifiables≤ | 15 | Q116-2002 |
| Free alkali NaOH≤ | 1.0 | GB/T260-77 |
| Moisture %≤ | 30 | SH/T0329 |
In oxidized petroleum waves saponification process, separated that remaining part is a unsaponifiables after the soap lye, unsaponifiables is under agitation condition, slowly add organic sour water or mineral acid, temperature of charge keeps 80 ± 5 ℃, stirred 40 minutes, adding sour terminal point, to be controlled at the material pH value be 3-2, static 1 hour of material separates waste liquid down from jar, and remaining yellow substance is for reclaiming wax, in the saponification jar, doubly measure clear warm water washing to reclaiming the wax adding, discharge waste water and interstitial impurity after static 1 hour, detect acid number after repeating 2 times at least, squeeze into that to reclaim the wax storage tank standby after qualified.
Embodiment 2
Paraffin, recovery wax are squeezed in the preheating can in 7: 3 ratios, impurities removal, Fen Shui, dewater and to be warming up to 120 ℃ of insulations standby, sylvite and manganese salt are by charging capacity 1.8 ‰, soda ash drops in the dissolving vessel by 0.6 ‰, add proper amount of clear water and the heating dissolve standby, get the caustic soda of inventory 50%, the alkaline solution of making concentration 28% is standby.The preparation of oxidized petroleum waves thereafter, saponification, refining and packaging step is identical with embodiment 1, mainly quality index is identical with embodiment 1, and is also identical with embodiment 1 to the processing of unsaponifiables.
Embodiment 3
Paraffin, recovery wax are squeezed in the preheating can in 8: 2 ratios, impurities removal, Fen Shui, dewater and to be warming up to 120 ℃ of insulations standby, sylvite and manganese salt are by charging capacity 2 ‰, soda ash drops in the dissolving vessel by 0.8 ‰, add proper amount of clear water and the heating dissolve standby, get the caustic soda of inventory 50%, the alkaline solution of making concentration 30% is standby.The preparation of oxidized petroleum waves thereafter, saponification, refining and packaging step is identical with embodiment 1, mainly quality index is identical with embodiment 1, and is also identical with embodiment 1 to the processing of unsaponifiables.
Claims (4)
1. process of producing oxygenated paraffin soap is characterized in that being made up of following steps:
(1). get the raw materials ready: a certain amount of paraffin is squeezed in the preheating can, impurities removal, Fen Shui, dewater and be warming up to 120 ℃ after the insulation standby, additive sylvite and manganese salt drop in the dissolving vessel by 0.3～0.8 ‰ by charging capacity 1.5～2 ‰, soda ash, it is standby to add water-solubleization back, get the caustic soda of inventory about 50%, make behind the alkaline solution of concentration 25-30% standby;
(2). the preparation of oxidized petroleum waves: the material that preheating in the preheating can is good is squeezed in the oxidizing tower, simultaneously by 40 cubic metres/tons per hour air quantity air feed in oxidizing tower, heat supply, catalyst solution is squeezed in the tower, when temperature of charge in the tower reaches 160 ± 2 ℃, begin to cause, kept 0.5 hour, wind supply quantity is brought up to 50 cubic metres/tons per hour, being cooled to 150 ± 2 ℃ begins to excite, after two hours, material is cooled to 120-130 ℃ in the tower, the beginning oxidation, wind supply quantity is increased to 60 cubic metres/tons per hour simultaneously, temperature-resistant, 80 cubic metres/tons per hour after 12 hours is brought up to air quantity in oxidation, temperature-resistant, begin to detect acid number after exciting end, when oxidizing tower material acid number reached 80-85mgKOH/g, oxidation finished, after oxidation finishes, material stops heat supply and is cooled to 120 ℃ in the tower, simultaneously wind supply quantity is reduced to 40 cubic metres/tons per hour, begins tower, material in the oxidizing tower is squeezed in the saponification jar that tankage 30-40%75 ℃ hot water is housed, will be reacted the oil-soluble acid that generates simultaneously and evenly squeeze into the saponification jar;
(3). saponification:
A. washing: the oxidized petroleum waves temperature that will squeeze into the saponification jar is adjusted to about 85 ℃, with steam or air, transfer to material and seethe state, when temperature of charge is lower than 85 ℃ in the saponification jar, stir with open steam, when being higher than 85 ℃, uses temperature of charge pneumatic blending instead, stirred at least 40 minutes, stirring stops the back and be incubated sedimentation under 85-90 ℃ of condition, sedimentation was discharged waste water and middle layer from the saponification pot bottom after 30 minutes, till detection washing rear oxidation cerinic acid value was slightly acidic to the waste water pH value, defective will the repetition washed;
B. saponification: the oxidized petroleum waves qualified to washing in the saponification jar, with being steam heated to 95-100 ℃, the water that adds inventory about 35% simultaneously under material boiling situation, adds the alkaline solution of getting ready in the oxidized petroleum waves, adding alkali number calculates by oxidized petroleum waves alkali charge=acid number per ton * 1.8 * 0.71 * 1.03 (excess base) ÷ concentration ÷ 1000, filled up the alkali after saponification 1 hour, the recirculation saponification is more than 1 hour, and saponification finishes back check pH value about 13, saponification is finished, otherwise continues alkaline saponification;
C. separate: after saponification finished, material insulation sedimentation was at least 3 hours in the saponification jar, and soap lye is squeezed into the soap lye storage tank, surpassed rest time to change next procedure again over to after 24 hours;
(4). refining: soap lye qualified in the storage tank is squeezed into tube furnace through pressure pump, adjust inlet amount and measure with fire, squeeze into during when material moisture and to be the oxidized paraffin wax soap work in-process in the treatment tank in 30% left and right sides, after check, adjust free alkali content, moisture, make it reach standard-required, material is qualified after testing in the treatment tank is finished product, and squeezes into the finished product jar and carry out metering packing.
2. process of producing oxygenated paraffin soap according to claim 1, it is characterized in that in the oxidized petroleum waves saponification process of described step 3, remainder after soap lye separates is a unsaponifiables, this unsaponifiables adds acid treatment under agitation condition, temperature of charge keeps 80 ± 5 ℃, stirred at least 40 minutes, adding sour terminal point, to be controlled at the material pH value be 3-2, and static at least 1 hour of material separates waste liquid down from jar, remaining yellow substance is for reclaiming wax, in the saponification jar, add the warm water washing, discharge waste water and interstitial impurity at least after static 1 hour, after the detection acid number is qualified reclaiming wax, it is standby to squeeze into recovery wax storage tank, detects defective repetition of acid number and washes.
3. process of producing oxygenated paraffin soap according to claim 1 is characterized in that the paraffin in the described step 1 replaces with partially recycled wax, wherein paraffin: reclaim wax in 6～8: 2～4 ratio adds.
4. according to claim 1 or 3 described process of producing oxygenated paraffin soap, it is characterized in that the adjustment of the free alkali in the described step 4,, add inventory 1% soda ash again for transferring to 0.8% with caustic soda soln earlier.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101346939A CN100485017C (en) | 2006-12-12 | 2006-12-12 | Process of producing oxygenated paraffin soap |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101346939A CN100485017C (en) | 2006-12-12 | 2006-12-12 | Process of producing oxygenated paraffin soap |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1974730A true CN1974730A (en) | 2007-06-06 |
| CN100485017C CN100485017C (en) | 2009-05-06 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101346939A Expired - Fee Related CN100485017C (en) | 2006-12-12 | 2006-12-12 | Process of producing oxygenated paraffin soap |
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| CN (1) | CN100485017C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103468316A (en) * | 2013-10-12 | 2013-12-25 | 福州大学 | Preparation method of high-acid saponified oxidized wax |
| CN104593072A (en) * | 2013-11-04 | 2015-05-06 | 中国石油化工股份有限公司 | Preparation process for oxidized paraffin |
-
2006
- 2006-12-12 CN CNB2006101346939A patent/CN100485017C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103468316A (en) * | 2013-10-12 | 2013-12-25 | 福州大学 | Preparation method of high-acid saponified oxidized wax |
| CN104593072A (en) * | 2013-11-04 | 2015-05-06 | 中国石油化工股份有限公司 | Preparation process for oxidized paraffin |
| CN104593072B (en) * | 2013-11-04 | 2016-02-10 | 中国石油化工股份有限公司 | A kind of processing method preparing oxidized petroleum wax |
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| Publication number | Publication date |
|---|---|
| CN100485017C (en) | 2009-05-06 |
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Application publication date: 20070606 Assignee: Beizhen Lufeng Chemical Factory Assignor: Liu Junsheng Contract record no.: 2013210000046 Denomination of invention: Process of producing oxygenated paraffin soap Granted publication date: 20090506 License type: Exclusive License Record date: 20130520 |
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