CN102910994A - Synthetic method of emulsifier SP-80 for emulsion explosive - Google Patents
Synthetic method of emulsifier SP-80 for emulsion explosive Download PDFInfo
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- CN102910994A CN102910994A CN2012104068682A CN201210406868A CN102910994A CN 102910994 A CN102910994 A CN 102910994A CN 2012104068682 A CN2012104068682 A CN 2012104068682A CN 201210406868 A CN201210406868 A CN 201210406868A CN 102910994 A CN102910994 A CN 102910994A
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Abstract
The invention discloses a synthetic method of an emulsifier SP-80 for an emulsion explosive. The synthetic method comprises the following steps: 1) etherifying sorbitol and a catalyst for 50-90 minutes at the temperature of 100-150 DEG C in a vacuum state to generate sorbitan anhydride; and 2) uniformly mixing the sorbitan anhydride, oleic acid and the basic catalyst, and esterifying for 2-5 hours at the temperature of 170-220 DEG C to generate the emulsifier SP-80 for the emulsion explosive as an early finished product. According to the synthetic method of the emulsifier SP-80 for the emulsion explosive, the problem of producing the SP-80 by a one-step method can be solved, the emulsifier SP-80 with excellent quality can be continuously and quickly produced by adopting a two-step method, and the produced emulsifier is higher in viscosity and is higher in hydroxyl value.
Description
Technical field
The present invention relates to a kind of synthetic method of emulsifying agent, the synthetic method of especially a kind of emulsifier for emulsion explosive SP-80.
Background technology
Develop emulsion explosive so far three during the last ten years from domestic, SP-80 as long-term a large amount of use of emulsifier in emulsion explosives, is the key ingredient of emulsion explosive always.The quality of SP-80 emulsifying agent directly affects the performance of emulsion explosive.At present, China SP-80 emulsifying agent manufacturer is a lot, although the emulsifying agent title is the same, be not quite similar with technique but feed intake during owing to reaction, it is larger that reaction product component differs, and causes the emulsion explosive performance of production very unstable, shelf lives is generally about 5 months, the sp-80 emulsifying agent of the manufacturer production that has can cause that explosive property decay in enormous quantities is very fast because of quality problems, and the meeting that has is miss-fired, thereby causes huge financial loss.
The Span-80 emulsifying agent is referred to as the Span-80 emulsifying agent, and its chemistry anhydrous sorbitol list olein by name is again emulsifying agent sp-80, belongs to a kind of of polyol-based non-ionic surfactant, and it is widely used in weaving, paint, oil, mining, medicine and the explosive.Particularly in the production of oil-in-water emulsify explosive, be widely used.The sp-80 emulsifying agent is to be combined to by sorbyl alcohol and oleic acid ester, and building-up reactions comprises the interior etherification reaction of sorbyl alcohol dehydration Cheng Huan, and anhydrous sorbitol and elaidin reaction generate the esterification of ester.Because synthesis technique is different, and the quality of the sp-80 that produces is just different, and because at present emulsifying agent production is hand control, produce extremely unstable, even thereby the difference of the same manufacturer production quality of criticizing emulsifying agent very large difference is also arranged.Adopt automatic control system, greatly reduce the unstable of production process, basically eliminate the mass discrepancies of different batch emulsifying agents.So select synthesis technique and the preparation method of production sp-80 emulsifying agent very important.
Produce in the past the sp-80 emulsifying agent and all adopted one-step technology production (being about to produce after sorbyl alcohol and two kinds of starting material of oleic acid are put in the reactor simultaneously), production technique falls behind, and production unit is aging, and the product performance index fluctuation is large, difficult quality guarantee, and production efficiency is low.Mainly there is following problem:
(1) temperature control is inaccurate in the material reaction process, and temperature rise rate is slow;
(2) vacuum pump efficient is not high, and pumping speed is low, and vacuum tightness can not reach production requirement;
(3) the reacting rear material cooling-down effect is poor, can not isolate product impurity fully, and product purity is inadequate;
(4) stirring velocity of reactor is lower, affects the homogeneity of material reaction.
(5) two kinds of materials heat up simultaneously and are unfavorable for the dehydration of sorbyl alcohol etherificate, and by product is many, and effective constituent is few.
Summary of the invention
Technical problem to be solved by this invention provides the synthetic method of a kind of emulsifier for emulsion explosive SP-80, can solve the problem of above-mentioned One-step production SP-80, the employing two-step approach is produced, can produce fast continuously superior in quality sp-80 emulsifying agent, the emulsifier viscosity of producing is slightly high, and hydroxyl value is slightly high.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is: the synthetic method of a kind of emulsifier for emulsion explosive SP-80, and this synthetic method may further comprise the steps:
1) with sorbyl alcohol and catalyzer under vacuum state, etherification reactions occur in 100～150 ℃, the reaction times is 50～90 minutes, generates the anhydrous sorbitol acid anhydride;
2) anhydrous sorbitol acid anhydride, insulation to 100～150 ℃ oleic acid and basic catalyst are mixed, in 170～220 ℃ of generation esterifications, the reaction times is 2～5 hours at vacuum state, generates just finished product of emulsifier for emulsion explosive SP-80.
This synthetic method also comprises:
3) emulsifier for emulsion explosive SP-80 head product is generated emulsifier for emulsion explosive SP-80 finished product after the precipitate and separate step.
In the step 1), the catalyzer of employing is phosphoric acid or phosphorous acid or tosic acid or ZnO, and the add-on of catalyzer is 0.5%～0.8% of sorbyl alcohol quality.
Step 2) in, the basic catalyst of employing is sodium hydroxide, and the add-on of basic catalyst is the 0.3%-0.7% of anhydrous sorbitol acid anhydride and oleic acid total mass.
Step 2) in, the quality of oleic acid is 150%～190% of sorbyl alcohol quality.
The present invention adopts two-step approach production, i.e. the synthetic emulsifier for emulsion explosive SP-80 of the dehydration of sorbyl alcohol etherificate and esterification is finished product just, and according to the synthesis technique requirement, at first the feed ratio of sorbyl alcohol and oleic acid must be accurately.According to the raw-material difference of different batches, can only in very little scope, adjust.When if the alkyd ratio is higher (in more satisfactory scope), the anhydrous sorbitol sesquialter fat in the esterification products, two fat, three fat are less, every detection qualified.If when the alkyd ratio is low (not in more satisfactory scope), the anhydrous sorbitol sesquialter fat in the esterification products, two fat, three fat increase, every detection index deviation is larger, can be defective.
Secondly the sorbyl alcohol degree of dehydration is very crucial.The producer's sorbyl alcohol intramolecular dehydration that has is not enough, will cause like this sorbitan monooleate effective constituent less, product yield is lower, the index hydroxyl value that characterizes out is too high, poor fluidity, the easy layering of product becomes newborn limiting quantity large, the product emulsifying capacity is low, thereby affects the quality product of emulsion explosive production.The producer's sorbyl alcohol intramolecular dehydration that has is excessive, carbonization phenomenon appears in sorbyl alcohol, it is darker that the product of producing will color and luster occur, viscosity is on the low side, and active constituent content reduces, although productive rate is higher and the flowability of emulsifying agent is better, but affected emulsifying capacity, the Quality of Emulsion Explosive of producing is relatively poor, affects the shelf lives, and performance degradation is fast especially.This just requires to select appropriate dehydration temperaturre, time and special catalyzer, and the dehydration of guarantee sorbyl alcohol is appropriate, thereby synthesizes superior in quality Sp-80 emulsifying agent, and wherein gordian technique is to select suitable catalyzer.
The synthetic temperature and time of esterification again.When synthetic, under the effect of basic catalyst, when being heated to certain temperature, an anhydrous sorbitol and two anhydrous sorbitols will generate with preheated oleic acid generation esterification reaction an anhydrous sorbitol olein and two anhydrous sorbitol oleins esterified.Temperature and time when regulating esterification can be controlled the ratio of an anhydrous sorbitol olein and two anhydrous sorbitol oleins.Producing the half-finished acid number of end precontract sampling half an hour detection, viscosity, determine reaction time of esterification according to detected result, accomplish controllability.
The synthetic method of a kind of emulsifier for emulsion explosive SP-80 provided by the invention, the employing two-step approach is produced, can realize automatic production control, produce fast continuously superior in quality sp-80 emulsifying agent, the emulsifier viscosity of producing is slightly high, hydroxyl value is slightly high, such emulsifying agent particularly suitable emulsion explosive production needs, and emulsifier is few, and dispersiveness and stability in storage are good, stability in storage can reach more than 6 months, and what have reached more than 1 year.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples:
Fig. 1 is synthesis process flow diagram of the present invention.
Embodiment
Embodiment 1
As shown in Figure 1, the synthetic method of a kind of emulsifier for emulsion explosive SP-80, this synthetic method may further comprise the steps:
1) with mass concentration be 70% sorbyl alcohol 13kg and catalyzer phosphoric acid under vacuum state (vacuum tightness is-0.075～0.085 MPa), etherification reactions occur in 120 ℃, the reaction times is 70 minutes, generates the anhydrous sorbitol acid anhydride;
2) anhydrous sorbitol acid anhydride, insulation to 120 ℃ oleic acid and basic catalyst are mixed, in 180 ℃ esterification occurs at vacuum state (vacuum tightness is-0.075～0.085 MPa), reaction times is 3.5 hours, generates just finished product of emulsifier for emulsion explosive SP-80;
3) with emulsifier for emulsion explosive SP-80 head product through adding the oxidation inhibitor precipitate and separate, generation emulsifier for emulsion explosive SP-80 finished product after the HLB value set-up procedure.
The phosphoric acid add-on is 0.5% of sorbyl alcohol quality in the step 1).
Step 2) in, the add-on of oleic acid is 150% of sorbyl alcohol quality, and the basic catalyst of employing is sodium hydroxide, and the add-on of basic catalyst is 0.3% of anhydrous sorbitol acid anhydride and oleic acid total mass.
The product kinetic viscosity (40 ℃) of the emulsifier for emulsion explosive SP-80 finished product of making: 1100mpa.s, acid number: 2.96mgKOH/g, saponification value: 156.38 mgKOH/g, hydroxyl value: 256.42mgKOH/g, moisture content: 0.12%, minimum critical amount emulsion test: 0.375%.
Embodiment 2
As shown in Figure 1, the synthetic method of a kind of emulsifier for emulsion explosive SP-80, this synthetic method may further comprise the steps:
1) with mass concentration be 70% sorbyl alcohol 13kg and catalyzer phosphorous acid under vacuum state (vacuum tightness is-0.075～0.085 MPa), etherification reactions occur in 125 ℃, the reaction times is 50 minutes, generates the anhydrous sorbitol acid anhydride;
2) anhydrous sorbitol acid anhydride, insulation to 125 ℃ oleic acid and basic catalyst are mixed, in 200 ℃ esterification occurs at vacuum state (vacuum tightness is-0.075～0.085 MPa), reaction times is 5 hours, generates just finished product of emulsifier for emulsion explosive SP-80;
3) with emulsifier for emulsion explosive SP-80 head product through adding the oxidation inhibitor precipitate and separate, generation emulsifier for emulsion explosive SP-80 finished product after the HLB value set-up procedure.
The phosphorous acid add-on is 0.6% of sorbyl alcohol quality in the step 1).
Step 2) in, the add-on of oleic acid is 160% of sorbyl alcohol quality, and the basic catalyst of employing is sodium hydroxide, and the add-on of basic catalyst is 0.5% of anhydrous sorbitol acid anhydride and oleic acid total mass.
The product kinetic viscosity (40 ℃) of the emulsifier for emulsion explosive SP-80 finished product of making: 450mpa.s, acid number: 3.56mgKOH/g, saponification value: 142.17 mgKOH/g, hydroxyl value: 192.33mgKOH/g, moisture content: 0.15%, minimum critical amount emulsion test: 0.5%.
Embodiment 3
As shown in Figure 1, the synthetic method of a kind of emulsifier for emulsion explosive SP-80, this synthetic method may further comprise the steps:
1) with mass concentration be 70% sorbyl alcohol 13kg and catalyzer tosic acid under vacuum state (vacuum tightness is-0.075～0.085 MPa), etherification reactions occur in 100 ℃, the reaction times is 80 minutes, generates the anhydrous sorbitol acid anhydride;
2) anhydrous sorbitol acid anhydride, insulation to 100 ℃ oleic acid and basic catalyst are mixed, in 220 ℃ esterification occurs at vacuum state (vacuum tightness is-0.075～0.085 MPa), reaction times is 4.5 hours, generates just finished product of emulsifier for emulsion explosive SP-80;
3) with emulsifier for emulsion explosive SP-80 head product through adding the oxidation inhibitor precipitate and separate, generation emulsifier for emulsion explosive SP-80 finished product after the HLB value set-up procedure.
The tosic acid add-on is 0.7% of sorbyl alcohol quality in the step 1).
Step 2) in, the add-on of oleic acid is 180% of sorbyl alcohol quality, and the basic catalyst of employing is sodium hydroxide, and the add-on of basic catalyst is 0.7% of anhydrous sorbitol acid anhydride and oleic acid total mass.
The product kinetic viscosity (40 ℃) of the emulsifier for emulsion explosive SP-80 finished product of making: 350mpa.s, acid number: 3.86mgKOH/g, saponification value: 141.22 mgKOH/g, hydroxyl value: 191.35mgKOH/g, moisture content: 0.18%, minimum critical amount emulsion test: 0.5%.
Embodiment 4
As shown in Figure 1, the synthetic method of a kind of emulsifier for emulsion explosive SP-80, this synthetic method may further comprise the steps:
1) with mass concentration be 70% sorbyl alcohol 13kg and catalyst Z nO under vacuum state (vacuum tightness is-0.075～0.085 MPa), etherification reactions occur in 150 ℃, the reaction times is 90 minutes, generates the anhydrous sorbitol acid anhydride;
2) anhydrous sorbitol acid anhydride, insulation to 150 ℃ oleic acid and basic catalyst are mixed, in 170 ℃ esterification occurs at vacuum state (vacuum tightness is-0.075～0.085 MPa), reaction times is 2 hours, generates just finished product of emulsifier for emulsion explosive SP-80;
3) with emulsifier for emulsion explosive SP-80 head product through adding the oxidation inhibitor precipitate and separate, generation emulsifier for emulsion explosive SP-80 finished product after the HLB value set-up procedure.
The tosic acid add-on is 0.8% of sorbyl alcohol quality in the step 1).
Step 2) in, the add-on of oleic acid is 190% of sorbyl alcohol quality, and the basic catalyst of employing is sodium hydroxide, and the add-on of basic catalyst is 0.6% of anhydrous sorbitol acid anhydride and oleic acid total mass.
The product kinetic viscosity (40 ℃) of the emulsifier for emulsion explosive SP-80 finished product of making: 500mpa.s, acid number: 2.94mgKOH/g, saponification value: 148.31 mgKOH/g, hydroxyl value: 206.37mgKOH/g, moisture content: 0.18%, minimum critical amount emulsion test: 0.5%.
Claims (5)
1. the synthetic method of an emulsifier for emulsion explosive SP-80 is characterized in that this synthetic method may further comprise the steps:
1) with sorbyl alcohol and catalyzer under vacuum state, etherification reactions occur in 100～150 ℃, the reaction times is 50～90 minutes, generates the anhydrous sorbitol acid anhydride;
2) anhydrous sorbitol acid anhydride, insulation to 100～150 ℃ oleic acid and basic catalyst are mixed, in 170～220 ℃ of generation esterifications, the reaction times is 2～5 hours at vacuum state, generates just finished product of emulsifier for emulsion explosive SP-80.
2. the synthetic method of a kind of emulsifier for emulsion explosive SP-80 according to claim 1 is characterized in that this synthetic method also comprises:
3) emulsifier for emulsion explosive SP-80 head product is generated emulsifier for emulsion explosive SP-80 finished product after the precipitate and separate step.
3. the synthetic method of a kind of emulsifier for emulsion explosive SP-80 according to claim 1 and 2, it is characterized in that: in the step 1), the catalyzer that adopts is phosphoric acid or phosphorous acid or tosic acid or ZnO, and the add-on of catalyzer is 0.5%～0.8% of sorbyl alcohol quality.
4. the synthetic method of a kind of emulsifier for emulsion explosive SP-80 according to claim 1 and 2, it is characterized in that: step 2) in, the basic catalyst that adopts is sodium hydroxide, and the add-on of basic catalyst is the 0.3%-0.7% of anhydrous sorbitol acid anhydride and oleic acid total mass.
5. the synthetic method of a kind of emulsifier for emulsion explosive SP-80 according to claim 1 and 2 is characterized in that: step 2) in, the quality of oleic acid is 150%～190% of sorbyl alcohol quality.
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| CN104909966A (en) * | 2015-06-30 | 2015-09-16 | 葛洲坝易普力湖北昌泰民爆有限公司 | Formula of composite oil phase for static emulsified and high-temperature sensitized emulsified explosive |
| CN105152820A (en) * | 2015-08-13 | 2015-12-16 | 陕西省汉阴华能新材料研究有限公司 | Emulsifier used for preparing explosives and preparation method of emulsifier |
| CN105859492A (en) * | 2016-04-01 | 2016-08-17 | 河南久联神威民爆器材有限公司 | Special compound oil phase for emulsion explosive and preparation method thereof |
| CN105949016A (en) * | 2016-05-12 | 2016-09-21 | 葛洲坝易普力湖北昌泰民爆有限公司 | Formula of compound oil phase for emulsion explosive emulsified in static state and sensitized at medium temperature and low temperature |
| CN106083497A (en) * | 2016-06-23 | 2016-11-09 | 湖北同石油化工有限公司 | A kind of LZ2735 emulsifying agent and preparation method thereof |
| CN106349197A (en) * | 2016-08-30 | 2017-01-25 | 荆门市燎原科技开发有限公司 | Preparing method of emulsifier Span-80 for emulsion explosive |
| CN106946818A (en) * | 2017-04-19 | 2017-07-14 | 杨桂廷 | The preparation method of emulsified explosive special emulsion agent |
| CN107670604A (en) * | 2017-10-16 | 2018-02-09 | 湖北东神天神实业有限公司 | A kind of emulsifier for emulsion explosive and its production method and production equipment |
| CN113024334A (en) * | 2021-03-24 | 2021-06-25 | 葛洲坝易普力湖北昌泰民爆有限公司 | Oil phase for preparing medium-low temperature sensitization process emulsion explosive by using coal-to-liquid intermediate product and preparation method thereof |
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| CN105152820A (en) * | 2015-08-13 | 2015-12-16 | 陕西省汉阴华能新材料研究有限公司 | Emulsifier used for preparing explosives and preparation method of emulsifier |
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| CN105949016A (en) * | 2016-05-12 | 2016-09-21 | 葛洲坝易普力湖北昌泰民爆有限公司 | Formula of compound oil phase for emulsion explosive emulsified in static state and sensitized at medium temperature and low temperature |
| CN106083497A (en) * | 2016-06-23 | 2016-11-09 | 湖北同石油化工有限公司 | A kind of LZ2735 emulsifying agent and preparation method thereof |
| CN106349197A (en) * | 2016-08-30 | 2017-01-25 | 荆门市燎原科技开发有限公司 | Preparing method of emulsifier Span-80 for emulsion explosive |
| CN106946818A (en) * | 2017-04-19 | 2017-07-14 | 杨桂廷 | The preparation method of emulsified explosive special emulsion agent |
| CN107670604A (en) * | 2017-10-16 | 2018-02-09 | 湖北东神天神实业有限公司 | A kind of emulsifier for emulsion explosive and its production method and production equipment |
| CN113024334A (en) * | 2021-03-24 | 2021-06-25 | 葛洲坝易普力湖北昌泰民爆有限公司 | Oil phase for preparing medium-low temperature sensitization process emulsion explosive by using coal-to-liquid intermediate product and preparation method thereof |
| CN113024334B (en) * | 2021-03-24 | 2022-04-22 | 葛洲坝易普力湖北昌泰民爆有限公司 | Oil phase for preparing medium-low temperature sensitization process emulsion explosive by using coal-to-liquid intermediate product and preparation method thereof |
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