CN101121783A - Method for preparing ethoxyabietic amine by spraying process - Google Patents

Abstract

The invention relates to a spray method to prepare the rosin amine polyoxyethylene; the reaction is divided into two steps: in the first step, the divergent rosin amine is absorbed into the spray reaction kettle; the material is heated until the temperature is between 50 and 60 Celsius system; the hypophosphite is inhaled; while vacuuming, the temperature is raised to be between 170 and 180 Celsius system; the pressure is controlled in the kettle to be between 0.2 and 0.3 Mpa; the vacuum valve is closed; the magnetic circulating pump is opened; the material is absorbed into the kettle and sprayed into the kettle; the valve of the ethylene oxide is opened; the material and the ethylene oxide are sprayed at the same time; such a cycle reaction is done for 0.8 to 1.5 hours; the temperature is kept for 30 to 40 minutes; the material is cooled until the temperature is between 90 and 100 Celsius system; in the second step, while vacuuming the kettle and absorbing the potassium hydroxide, the temperature is raised to be between 120 and 130 Celsius system; the temperature is kept for more than 20 minutes; the air is replaced in the kettle with the nitrogen; the temperature is raised to be between 165 and 175 Celsius system; the vacuum valve is closed; the magnetic circulating pump is opened; the material and the left ethylene oxide are sprayed into the spray-typed reaction kettle at the same time; such a cycle reaction is done for 1 to 2 hours; the temperature is kept for more than 40 minutes. In the method of the invention, the reaction time is short and the reaction is complete; the matching and dissolvability of the compound with other surfactants are good.

Description

Spray method prepares the method for rosin Amine D Soxylat A 25-7

Technical field

The present invention relates to the method that a kind of spray method prepares the rosin Amine D Soxylat A 25-7.Belong to the chemical assistant technical field.

Background technology

The rosin Amine D Soxylat A 25-7 is widely used in Chemical Manufacture and makes emulsifying agent.The preparation method of rosin Amine D Soxylat A 25-7 mostly adopts paddling process at present: it is to be prepared by addition reaction in the stirring-type reactor by disproportionated rosin amine and oxyethane.Catalyzer is basic catalyst and an acidic catalyst.The polymerization reactant of this method rosin Amine D and oxyethane transforms not exclusively, and the polyreaction space is little, and polyreaction is subjected to the influence of material big, the contained viscosity of product primary, unhindered amina such as secondary amine is more, reaction not exclusively, not thorough.And the reaction times is longer, the finished product inferior quality.Behind the rosin Amine D Soxylat A 25-7 and other surfactant compounds with the paddling process preparation, can produce a lot of flosss, poor stability mixes.

Summary of the invention

The objective of the invention is to overcome above-mentioned deficiency, provide short, the reaction of a kind of reaction times thoroughly, prepare the method for rosin Amine D Soxylat A 25-7 with the good spray method of other surfactant compound intermiscibilities.

The object of the present invention is achieved like this: a kind of spray method prepares the method for rosin Amine D Soxylat A 25-7, it is to be raw material with the disproportionated rosin amine, add an acidic catalyst and basic catalyst and oxyethane and carry out polyreaction, it is characterized in that: adopt spray method, divide secondary to add catalyzer, reaction divided for two steps carried out:

The first step, disproportionated rosin amine is sucked in the spraying type reactor, when being heated to 50-60 ℃, suck phosphorous acid, be warming up to 170-180 ℃ while vacuumizing, control still internal pressure 0.2-0.3Mpa, close vacuum valve, open the magnetic force recycle pump, material is sprayed in the still by sucking-off in the still again, opens the valve of logical oxyethane, material and oxyethane are sprayed simultaneously by many groups combined sprinkler of spraying type reactor, sheaf space carries out spray reaction in still, and so circulating reaction 0.8-1.5 hour, the add-on of oxyethane accounted for its 10-30% that adds total amount, reaction finishes insulation 30-40 minute, is cooled to 90-100 ℃;

Second goes on foot, vacuumizes at above-mentioned spray reaction still inner edge, and the limit sucks potassium hydroxide, and the limit is warming up to 120-130 ℃, insulation with air in the nitrogen replacement still, was warmed up to 165-175 ℃ more than 20 minutes, close vacuum valve, open the magnetic force recycle pump, material and remaining oxyethane spray into the spraying type reactor simultaneously by many groups combined sprinkler of spraying type reactor, so circulating reaction 1-2 hour, when decompression occurring in the still, show that reaction process finishes, be incubated more than 40 minutes cooling discharging.

The present invention adopts the quadric catalysis two step method to produce, the first step is carried out polymerization adding under the acid catalyst situation, can allow disproportionated rosin amine and oxyethane under the condition of the temperature and pressure of setting, better carry out the amine ethoxylation, it is to generate a series of primary, secondary, uncle by mixture that different rings oxidative ethane adduction is counted reaction result, under the effect of acid catalyst, unsaturated primary amine, secondary amine are thoroughly opened, under the oxyethane effect, optionally generate tertiary amine, react better when making its polymerization.Second step made the material molecular structure form the liposuction space after adding alkaline catalysts, and its surface-area is significantly increased, and the molecular surface state is a tridimensional network, has good thixotroping and dispersing property.

The present invention adopts soda acid two-stage catalysis method, and promptly first selectivity is synthesized N, N-dihydroxy ethyl tertiary amine, and carbon catalyzing and synthesizing amine Soxylat A 25-7 on this basis then, the polyoxyethylene groups tertiary amine of synthetic product solid content 〉=95% makes polyreaction more thorough.

The present invention adopts spray polymerization technology, from suction, to vacuumize, temperature reaction, cooling, the discharging all processes all carries out in successive polymerization spray reaction still and control and finish, reaction atomizing effect, reaction times are regulated and control by many groups combined sprinkler is artificial, the material reaction compartment that atomizes in still is big, the material reaction contact area is big, and reaction thoroughly, and is effective, reaction times shortens 2-3 hour than paddling process, the product physical and chemical index is stable, and is easy to operate, safe and reliable.The present invention is hydrophilic good, and active matter content 〉=95% is used under 8 moles of ethylene oxide conditions of the present invention, can surpass the solvability in solution such as water, acid, alkali of the oxyethane of 10 moles of paddling process.

Rosin Amine D Soxylat A 25-7 product performance by the spray polymerization method preparation of two step of above-mentioned quadric catalysis are good, carry out compositely with itself and various tensio-active agent, have good composite intermiscibility, and result of use is splendid, and specific performance sees the following form:

Two step of quadric catalysis spray method polymerization technique stirs polymerization technique technical feature contrast table with tradition

Index name	Two step of quadric catalysis spray art	The tradition stirring technique
			Cloud point	RA8Eo 44～48℃	RA10Eo 70～72℃
Viscosity mpa.s	68.63	147.16
			Detersive power %	45.59	35.46
The HLB value	≥10	≤8
			Compatibility	Good	Difference
Floss	Do not have	Have
			Emulsifying property	Excellent	Very
Water-soluble	Good with the water dissolubility	Poor with the water dissolubility
			Solid content	≥95％	≥89％
Processing conditions	Polymerization time 4h, easy to operate	Polymerization time 7h, not easy to operate
			The security of equipment	Reliably	Difference

Embodiment

The present invention relates to the method that a kind of spray method prepares the rosin Amine D Soxylat A 25-7, it is to be raw material with the disproportionated rosin amine, adds an acidic catalyst and basic catalyst and oxyethane and carries out polyreaction, adopts spray method, divide secondary to add catalyzer, reaction divided for two steps carried out.

Embodiment 1:

The first step, in 2000L spraying type reactor, suck disproportionated rosin amine 580kg, when being heated to 50 ℃, suck the phosphorous acid 1.5kg of 70% (wt), be warming up to 170 ℃ while vacuumizing, control still internal pressure 0.3Mpa, close vacuum valve, open the magnetic force recycle pump, material is sprayed in the still by sucking-off in the still again, opens the valve of logical oxyethane, material and oxyethane are sprayed simultaneously by many groups combined sprinkler of spraying type reactor, sheaf space carries out spray reaction in still, and so circulating reaction is 1.2 hours, the add-on 120kg of oxyethane, reaction finishes insulation 30 minutes, is cooled to 95 ℃;

Second goes on foot, vacuumizes at above-mentioned spray reaction still inner edge, the limit sucks the potassium hydroxide 4kg of 50% (wt), the limit is warming up to 125 ℃, insulation is more than 30 minutes, continuous quadratic air in the nitrogen replacement still, be warmed up to 165 ℃, close vacuum valve, open the magnetic force recycle pump, material and remaining oxyethane 1080kg spray into the spraying type reactor simultaneously by many groups combined sprinkler of spraying type reactor, and so circulating reaction is 1.3 hours, when decompression occurring in the still, show that reaction process finishes, and is incubated 40 minutes, cooling discharging.

Embodiment 2:

The first step, in 2000L spraying type reactor, suck disproportionated rosin amine 580kg, when being heated to 60 ℃, suck the phosphorous acid 1.5kg of 70% (wt), be warming up to 180 ℃ while vacuumizing, control still internal pressure 0.2Mpa, close vacuum valve, open the magnetic force recycle pump, material is sprayed in the still by sucking-off in the still again, opens the valve of logical oxyethane, material and oxyethane spray during by many groups group shower nozzle contract of spraying type reactor, sheaf space carries out spray reaction in still, and so circulating reaction is 0.8 hour, the add-on 240kg of oxyethane, reaction finishes insulation 35 minutes, is cooled to 100 ℃;

Second goes on foot, vacuumizes at above-mentioned spray reaction still inner edge, the limit sucks the potassium hydroxide 4kg of 50% (wt), the limit is warming up to 130 ℃, insulation is more than 40 minutes, continuous three times with air in the nitrogen replacement still, be warmed up to 170 ℃, close vacuum valve, open the magnetic force recycle pump, material and remaining oxyethane 960kg spray into the spraying type reactor simultaneously by many groups combined sprinkler of spraying type reactor, and so circulating reaction is 2 hours, when decompression occurring in the still, show that reaction process finishes, and is incubated 40 minutes, cooling discharging.

Embodiment 3:

The first step, in 2000L spraying type reactor, suck disproportionated rosin amine 480kg, when being heated to 55 ℃, the phosphorous acid 1.5kg of 70% (wt), be warming up to 175 ℃ while vacuumizing, control still internal pressure 0.25Mpa, close vacuum valve, open the magnetic force recycle pump, material is sprayed in the still by sucking-off in the still again, opens the valve of logical oxyethane, material and oxyethane are sprayed simultaneously by many groups combined sprinkler of spraying type reactor, sheaf space carries out spray reaction in still, and so circulating reaction is 1.5 hours, the add-on 360kg of oxyethane, reaction finishes insulation 40 minutes, is cooled to 90 ℃;

Second goes on foot, vacuumizes at above-mentioned spray reaction still inner edge, the limit sucks the potassium hydroxide 4kg of 50% (wt), the limit is warming up to 120 ℃, insulation is more than 40 minutes, continuous quadratic air in the nitrogen replacement still, be warmed up to 175 ℃, close vacuum valve, open the magnetic force recycle pump, material and remaining oxyethane 840kg spray into the spraying type reactor simultaneously by many groups combined sprinkler of spraying type reactor, and so circulating reaction is 1 hour, when decompression occurring in the still, show that reaction process finishes, and is incubated 40 minutes, cooling discharging.

Claims (1)

1. a spray method prepares the method for rosin Amine D Soxylat A 25-7, it is to be raw material with the disproportionated rosin amine, adds an acidic catalyst and basic catalyst and oxyethane and carries out polyreaction, it is characterized in that: adopt spray method, divide secondary to add catalyzer, reaction divided for two steps carried out:

The first step, disproportionated rosin amine is sucked in the spraying type reactor, when being heated to 50-60 ℃, suck phosphorous acid, be warming up to 170-180 ℃ while vacuumizing, control still internal pressure 0.2-0.3Mpa, close vacuum valve, open the magnetic force recycle pump, material is sprayed in the still by sucking-off in the still again, opens the valve of logical oxyethane, material and oxyethane are sprayed simultaneously by many groups combined sprinkler of spraying type reactor, sheaf space carries out spray reaction in still, and so circulating reaction 0.8-1.5 hour, the add-on of oxyethane accounted for its 10-30% that adds total amount, reaction finishes insulation 30-40 minute, is cooled to 90-100 ℃;

Second goes on foot, vacuumizes at above-mentioned spray reaction still inner edge, and the limit sucks potassium hydroxide, and the limit is warming up to 120-130 ℃, insulation with air in the nitrogen replacement still, was warmed up to 165-175 ℃ more than 20 minutes, close vacuum valve, open the magnetic force recycle pump, material and remaining oxyethane spray into the spraying type reactor simultaneously by many groups combined sprinkler of spraying type reactor, so circulating reaction 1-2 hour, when decompression occurring in the still, show that reaction process finishes, be incubated more than 40 minutes cooling discharging.