CN105037144A - 2-ethylexanoic acid bi-trimethylolpropane ester and production method thereof - Google Patents

Abstract

The invention discloses 2-ethylexanoic acid bi-trimethylolpropane ester and a preparation method thereof. The molecular formula of the 2-ethylexanoic acid bi-trimethylolpropane ester is C44H82O9 and the structural formula of the 2-ethylexanoic acid bi-trimethylolpropane ester is as shown in the specification. The preparation method comprises the following steps: as for bi-trimethylolpropane and 2-ethylexanoic acid purchased in current batch, firstly, determining a theoretic molar ratio required in complete esterification reaction with the 2-ethylexanoic acid according to the quantity of hydroxyls in bi-trimethylolpropane molecules, or carrying out multiple pilot tests according to an empirical molar ratio formed with regard to such raw materials previously; when a sample subjected to current pilot test meets conditions, ending the test, and carrying out production by taking the raw material batch and the raw material ratio of the last pilot test as the raw material ratio of large-scale production. The 2-ethylexanoic acid bi-trimethylolpropane ester and the preparation method have the advantage that raw materials are sufficiently utilized and the troubles of product posttreatment are reduced by the adoption of the 2-ethylexanoic acid bi-trimethylolpropane ester preparation technology.

Description

2 ethyl hexanoic acid ditrimethylolpropane ester and a kind of production method thereof

Technical field

The invention belongs to organic chemistry raw material and manufacture field, disclose the 2 ethyl hexanoic acid ditrimethylolpropane ester that a kind of ditrimethylolpropane and 2 ethyl hexanoic acid are obtained by esterification, also relate to a kind of preparation technology of 2 ethyl hexanoic acid ditrimethylolpropane ester.

Background technology

In numerous fatty acid esters, a class fatty acid ester is had to have the special construction of quaternary carbon atom, also known as neopentyl structure, typical example as: pentaerythritol fatty ester, bis pentaervthritol ester, trimethylolpropane fatty acid ester, ditrimethylolpropane fatty acid ester, neopentyl glycol fatty acid ester, they enjoy the favor of people.Because the β position carbon atom of the carbonyl of these neo-pentyl fatty acid esters does not have hydrogen atom, so can not with the resonance structure of the carbon of the alcohol moiety of ester group and hydrogen evolution six atom cycloalkyl, only have high-energy could destroy such ester structure, this makes the stability of the oxidation-resistance of amyl-based polyol fatty acid ester and anti-elimination reaction fine.Thus amyl-based polyol fatty acid ester has the unrivaled superiority of other ester class, becomes the optimal selection of the high-end synthetic ester in current lubricating oil.

Not only thermal oxidation stability is good for amyl-based polyol fatty acid ester, heat decomposition temperature is high, and resistance to low temperature good, easily degrade in the environment, the lubricant in the synthetic base oil of lubricating oil and metal rolled process can be used as, so be more and more subject to people's attention.

Although people have synthesized numerous amyl-based polyol fatty acid esters, but it is little to the report synthesizing 2 ethyl hexanoic acid ditrimethylolpropane ester to carry out esterification with ditrimethylolpropane (also known as two-TriMethylolPropane(TMP), Di-trimethylolpropane) and 2 ethyl hexanoic acid under the effect of an acidic catalyst.

Ditrimethylolpropane is a kind of compound having four alcoholic extract hydroxyl groups, have neopentyl structure.It is unlike tetramethylolmethane, and its alcoholic extract hydroxyl group is not connected on a carbon atom, forms the molecule of stereo structure, but is dispersed on two carbon atoms, thus can form the molecule of flush type after being unlikely to carry out esterification with acid.Because the molecular weight of ditrimethylolpropane is larger, so although there is higher viscosity with the amyl-based polyol fatty acid ester that ditrimethylolpropane synthesizes, but the steric effect in molecule is not clearly, can be applied to the occasion needing high viscosity lubricants.

2 ethyl hexanoic acid is a kind of common, saturated fatty acid of being easy to get, and because it is branched acid, so not only the zero pour of itself is lower, and it is also lower with the pour point of its amyl-based polyol fatty acid ester synthesized, make product not only can be high temperature resistant, and can be low temperature resistant, be in liquid wider range.Synthesize the synthetic ester obtained with saturated fatty acid, its oxidation resistant stability also can be relatively good.

The technique document of current synthesis amyl-based polyol fatty acid ester series products is many, nothing more than employing direct esterification and ester-interchange method.Ester-interchange method owing to using basic catalyst, and can produce lower aliphatic alcohols etc. and has inflammable and byproduct that is explosion hazard, so in fact use seldom.Even employing direct esterification, be mostly adopt the excessive reaction forward of impelling of certain raw material to carry out, this will run into excessive raw material and the difficulty of product separation in follow-up purification, treating process.Even if adopt the means such as molecule rectifying to remove certain excessive raw material, even if can take off very thorough, also will inevitably cause the decline of target product yield, and the energy consumption that sepn process brings thus also can not be ignored, be thus difficult to synthesize the competitive product of price.

The current production technique display of some document reflection, in the process of synthesis amyl-based polyol fatty acid ester, adopts solvent or water entrainer to improve the efficiency of dehydration, makes esterification be unlikely to just can carry out at relatively high temperatures thoroughly.But one that adopts such technique to bring fearful effect finally will allow these solvents or water entrainer and product realize being separated thoroughly also very difficult.And the existence of a small amount of low boiling point solvent or water entrainer can cause the flash-point of product obviously to decline, at high temperature use to product and bring hidden danger.

The also current production technique display of some document reflection, in order to improve esterification yield, reduce the time of reaction, often adopts the excessive way of lipid acid to react, then carries out aftertreatment to product.To in the aftertreatment of product, mostly adopt neutralization, washing and point equal purification means.The consequence adopting such technology to bring is that the raw material of these acidity has loss, unit consumption is difficult to reach desirable level, production cost remains high.The salt produced in N-process is difficult to removing, and the process that will meet environmental requirement to the salt be in waste water is also a thing that make repeated headache.Because used alkaline matter in the process of aftertreatment, there is the situation of saponification reaction in the ester that also may occur to be synthesized, product is gone wrong again in follow-up use procedure.

Double the disclosed process data about synthetic ester, can find in current Technology in the selection of catalyzer, mostly the catalyzer of abandoning tradition, use load miscellaneous or composite catalyst instead.The cost in fact preparing various novel catalyzer is just higher, and the catalytic effect of these novel catalyzer is good not as good as traditional catalyst.Even if some solid catalyst can reclaim, but along with the effective constituent of in use solid-carried catalyst is constantly by wash-out, in fact these catalyzer can reusable restricted lifetime.

Because the source of raw material is different, production technique is also not quite similar, the index such as purity, foreign matter content of different batches raw material also exists trickle fluctuation, so qualified amyl-based polyol fatty acid ester will be produced, also need the feature for different batches raw material to carry out lab scale to grope, the proportioning of Reasonable adjustment raw material.

For the quality fluctuation of raw material between the deficiency of existing production amyl-based polyol fatty acid ester Product Process and different batches, be necessary the harmony considered production control cost and take into account quality product, adopt the tosic acid be easy to get as catalyzer, in conjunction with determining rational proportioning between different batches raw material by lab scale, come economical, reasonably produce 2 ethyl hexanoic acid ditrimethylolpropane ester.

Summary of the invention

The object of the invention is to disclose the 2 ethyl hexanoic acid ditrimethylolpropane ester that a kind of ditrimethylolpropane and 2 ethyl hexanoic acid are obtained by esterification, also providing a kind of adopts tosic acid to be catalyzer, in conjunction with adjusting, determining rational proportioning between different batches raw material by lab scale, the preparation technology of 2 ethyl hexanoic acid ditrimethylolpropane ester economically and reasonably.

For solving the problems of the technologies described above, technical scheme of the present invention is: 2 ethyl hexanoic acid ditrimethylolpropane ester, and its innovative point is: its molecular formula is C ₄₄h ₈₂o ₉, there is structural formula as follows:

A preparation method for above-mentioned 2 ethyl hexanoic acid ditrimethylolpropane ester, its innovative point is: the corresponding reaction equation of described preparation technology is as follows:

For ditrimethylolpropane and the 2 ethyl hexanoic acid of purchasing the present lot come, first determine the theoretical molar proportioning of carrying out with 2 ethyl hexanoic acid completely needed for esterification according to the quantity of hydroxyl in ditrimethylolpropane molecule used, or select the mol ratio of current lab scale according to the former experience mol ratio formed for ditrimethylolpropane and 2 ethyl hexanoic acid;

Adopt tosic acid as catalyzer, rely on heating to carry out esterification when logical nitrogen, and the water taken out of with nitrogen is collected by collection device, observe in collection device and no longer included after water deviates from 5 ~ 20 minutes, sampling, the acid number of working sample, makes current lab scale sample meet acid number≤1.5mgKOH/g by the adjustment of one or many lab scale mol ratio;

Add gac, continue heated and stirred 0.5 ~ 2h, then heating is stopped, when being cooled to 50 ~ 70 DEG C in lab scale sample, suction filtration is carried out while hot in the Büchner funnel being covered with diatomite and middling speed quantitative paper, product in filter flask is transferred in reagent bottle, the method specified according to GB/T7305-2003, measure the separation property of synthesis liquid and water; After if the result display high-speed stirring recorded terminates within three ten minutes left standstill after, the volume of emulsion layer is less than 3mL, then represent that the separation property of this synthesis liquid and water is good, terminate this lab scale;

Acid number≤1.5mgKOH/g in this lab scale and synthesis liquid and water separation property also satisfactory lab scale mol ratio carry out large-scale production as the proportioning raw materials of present lot raw material.

Further, described concrete steps are as follows:

step S1: for ditrimethylolpropane and the 2 ethyl hexanoic acid of purchasing the present lot come, the quantity calculating hydroxyl in ditrimethylolpropane molecule used determines the theoretical molar proportioning of carrying out with 2 ethyl hexanoic acid completely needed for esterification, or the mol ratio of current lab scale was selected according to the former experience mol ratio formed for ditrimethylolpropane and 2 ethyl hexanoic acid, the hydroxyl value of a part ditrimethylolpropane is 4, so 2 ethyl hexanoic acid is 4 with the theoretical molar ratio of ditrimethylolpropane;

step S2:the mol ratio setting ditrimethylolpropane and 2 ethyl hexanoic acid in this lab scale is 0.9:4 ~ 1.3:4;

step S3:carry out lab scale, in the three-necked bottle of 500mL, first put into magnetic stir bar, drop into the 2 ethyl hexanoic acid of 0.8 ~ 2.0mol, then the ditrimethylolpropane meeting the respective batch that mol ratio requires in step S2 is dropped into, open the intensification switch of oil bath heater, material in still is heated, when temperature in the kettle is raised to 110 ± 4 DEG C, add 2 ethyl hexanoic acid and ditrimethylolpropane always feed intake quality 0.5 ~ 2% tosic acid as catalyzer, under nitrogen tube is inserted into liquid level, nitrogen is passed into the flow velocity of 10 ~ 100mL/min, open the stirring of stirrer in magnetic agitation still, timing from now, material in still is warmed up to 140 ~ 200 DEG C, heating 10 ~ 24h, the water of observing response by-product is deviate to the speed conditions in collection device under the drive of nitrogen, by the time no longer included after a water deviates from collection device in 5 ~ 20 minutes, sampling,

step S4:the acid number of working sample, if the acid number≤1.5mgKOH/g of sample, then leaps to step S9; If the acid number > 1.5mgKOH/g of sample, then enter next step;

step S5:continue reaction 0.5 ~ 2h;

step S6:the reacted acid number of sampling and measuring, if acid number≤1.5mgKOH/g, then jumps to step S9; If acid number > is 1.5mgKOH/g, then enter next step;

step S7:judge the absolute value of acid number and the adjacent last hypo acid value difference measured in above-mentioned steps S6, if this absolute value > is 0.5mgKOH/g, then return step S5; If this absolute value≤0.5mgKOH/g, then enter next step;

step S8:if acid number is > 1.5mgKOH/g still, then terminate this lab scale, and return step S2, again adjust in the scope of 0.9:4 ~ 1.3:4 and set once the concrete mol ratio of 2 ethyl hexanoic acid and ditrimethylolpropane in lab scale test; If acid number≤1.5mgKOH/g, then enter next step;

step S9:add in three-necked bottle ditrimethylolpropane and 2 ethyl hexanoic acid always feed intake quality 0.5 ~ 2% gac, continue heated and stirred 0.5 ~ 2h, then heating is stopped, when being cooled to 50 ~ 70 DEG C in lab scale sample, in the Büchner funnel being covered with diatomite and middling speed quantitative paper, carry out suction filtration while hot, the product in filter flask is transferred in reagent bottle;

step S10:according to the method that GB/T7305-2003 specify, synthesis liquid in mensuration reagent bottle and the separation property of water, if be less than 3mL at the volume of the three ten minutes internal emulsification layers left standstill after the result display high-speed stirring recorded terminates, then represent that the separation property of this synthesis liquid and water is good, terminate this lab scale, write down this batch of ditrimethylolpropane and the suitable mol ratio of 2 ethyl hexanoic acid, using the mol ratio of this lab scale as proportioning raw materials when carrying out large-scale production with the raw material of present lot; If the separation property of measurement result display synthesis liquid and water is bad, then return step S2 ,in the test of fine setting lab scale, the concrete mol ratio of 2 ethyl hexanoic acid and ditrimethylolpropane, then carries out lab scale next time;

step S11:large-scale production;

Further, the step of described large-scale production is specially:

step S111:the ditrimethylolpropane for present lot obtained with lab scale and the suitable mol ratio of 2 ethyl hexanoic acid, at 1M ³reactor in, drop into 2 ethyl hexanoic acid and ditrimethylolpropane, the total mass of raw material in still is made to be in the scope of 200 ~ 700kg, open and stir, during beginning, rotating speed maintains 5 ~ 50rpm, open the heating valve of reactor, material in still is heated, when temperature in the kettle is raised to 115 ± 5 DEG C, add 2 ethyl hexanoic acid and ditrimethylolpropane always feed intake quality 0.5 ~ 2% tosic acid as catalyzer, open nitrogen valve, nitrogen is passed into the flow velocity of 1 ~ 100L/min, the rotating speed of stirring is brought up to 50 ~ 300rpm, timing from now, material in still is warmed up to 140 ~ 200 DEG C, heating 10 ~ 24h, the water of observing response by-product is deviate to the speed conditions in collection device under the drive of nitrogen, by the time no longer included after a water deviates from collection device in 5 ~ 20 minutes, sampling, the acid number of working sample,

step S112:if the acid number of sample can not reach≤level of 1.5mgKOH/g, then carry out reaction 0.5 ~ 2h, resampling detects acid number, until the acid number≤1.5mgKOH/g of sample;

step S113:add in reactor ditrimethylolpropane and 2 ethyl hexanoic acid always feed intake quality 0.1 ~ 2% gac, the diatomite of 0.1 ~ 1%, continue heated and stirred 0.5 ~ 3h, then heating is stopped, when being cooled to 50 ~ 70 DEG C Deng the temperature of product in still, open the valve at the bottom of still, with refining filtering pump by flow out material pumping in pressure filter, carry out circulation press filtration, press filtration material out turns back in reactor, till the color that circulation press filtration proceeds to the product returned has not seen that the activated carbon granule of diatomite particle and black is residual, product after press filtration being decoloured pours in pail pack.

The invention has the advantages that:

(1) 2 ethyl hexanoic acid ditrimethylolpropane ester of the present invention, for the lurid thick liquid of one, owing to being adopt ditrimethylolpropane and 2 ethyl hexanoic acid through esterification, and both mol ratio are close to the such theoretical molar proportioning of 1:4, infer so corresponding amyl-based polyol fatty acid ester can be synthesized according to the amyl-based polyol adopting in the industry other similar and similar fatty acid ester, the main component of such product should be 2 ethyl hexanoic acid ditrimethylolpropane ester, and its molecular formula is C ₄₄h ₈₂o ₉, this 2 ethyl hexanoic acid ditrimethylolpropane acid esters can be used as degradable lubricant base and lubricant.

(2) each batch of raw material owing to buying has trickle fluctuation in purity, so adopt in the theoretical molar proportioning of corresponding raw material or the basis of experience mol ratio, the raw material of each batch is first adjusted to their proportioning by lab scale, until the acid number of amyl-based polyol fatty acid ester that lab scale is synthesized both met the requirements, also after meeting the requirements with the separation property of water, the feed molar proportioning adopting this suitable again goes to carry out large-scale production, raw material can be made to be fully utilized, ensure the quality of product, eliminate the highly energy-consuming that molecule rectifying is such, the lossy post-processing step of product, make production process economy, rationally, product has the market competitiveness.

(3) need not as current some processes, high, the not poisonous organic solvent of the boiling point such as toluene, dimethylbenzene is adopted to go as water entrainer, avoid the Dangerous and Harmful Factors in operating process, there is not the residual of low-boiling-point substance in product, thus ensure that the amyl-based polyol fatty acid ester be synthesized can at high temperature use.

(4) lipid acid owing to not adopting some traditional technologys to adopt is excessive, and then the technique that neutralizes is carried out with alkaline solution, eliminate washing and point equal post-processing step, and reluctant salts substances can not be produced, make that production process seems succinctly, environmental protection, avoid the product that is synthesized in the basic conditions again by the risk of saponification, hydrolysis.

(5) adopt traditional tosic acid as catalyzer, conveniently be easy to get, not exist batch between the discrepant problem of catalytic activity, it also has a benefit, be exactly that its fusing point is about 106 DEG C, after reaction end product cools down, in the process of decolorization filtering, the tosic acid of separating out from system can be filtered out together, realize being separated of catalyzer and product.

(6) gac and diatomite is adopted to combine as adsorption decolouriser, can the rational thickness of filter bed of heap, under the prerequisite of quality of guaranteeing to decolour, reduce the consumption of price greater activity charcoal, effectively reduce the cost of decolorization.

Embodiment

The invention discloses a kind of 2 ethyl hexanoic acid ditrimethylolpropane ester, its molecular formula is C ₄₄h ₈₂o ₉, there is structural formula as follows:

The corresponding reaction equation of preparation method also disclosing a kind of above-mentioned 2 ethyl hexanoic acid ditrimethylolpropane ester is as follows:

For ditrimethylolpropane and the 2 ethyl hexanoic acid of purchasing the present lot come, first determine the theoretical molar proportioning of carrying out with 2 ethyl hexanoic acid completely needed for esterification according to the quantity of hydroxyl in ditrimethylolpropane molecule used, or select the mol ratio of current lab scale according to the former experience mol ratio formed for ditrimethylolpropane and 2 ethyl hexanoic acid;

Adopt tosic acid as catalyzer, rely on heating to carry out esterification when logical nitrogen, and the water taken out of with nitrogen is collected by collection device, observe in collection device and no longer included after water deviates from 5 ~ 20 minutes, sampling, the acid number of working sample, makes current lab scale sample meet acid number≤1.5mgKOH/g by the adjustment of one or many lab scale mol ratio;

Add gac, continue heated and stirred 0.5 ~ 2h, then heating is stopped, when being cooled to 50 ~ 70 DEG C in lab scale sample, suction filtration is carried out while hot in the Büchner funnel being covered with diatomite and middling speed quantitative paper, product in filter flask is transferred in reagent bottle, the method specified according to GB/T7305-2003, measure the separation property of synthesis liquid and water; After if the result display high-speed stirring recorded terminates within three ten minutes left standstill after, the volume of emulsion layer is less than 3mL, then represent that the separation property of this synthesis liquid and water is good, terminate this lab scale;

Acid number≤1.5mgKOH/g in this lab scale and synthesis liquid and water separation property also satisfactory lab scale mol ratio carry out large-scale production as the proportioning raw materials of present lot raw material.

The following examples can make the present invention of professional and technical personnel's comprehend, but therefore do not limit the present invention among described scope of embodiments.

embodiment 1

step S1:for ditrimethylolpropane and the 2 ethyl hexanoic acid of purchasing the present lot come, have 4 hydroxyls in a ditrimethylolpropane molecule, then 2 ethyl hexanoic acid is 4 with the theoretical molar ratio of ditrimethylolpropane;

step S2:set the mol ratio of 2 ethyl hexanoic acid and ditrimethylolpropane in this lab scale, the theoretical molar proportioning 1:4 of both employings carries out lab scale test;

step S3:carry out lab scale, in the three-necked bottle of 500mL, first put into magnetic stir bar, drop into 1.2mol(173.052g) 2 ethyl hexanoic acid, then correspondingly drop into 0.3mol(75.099g) ditrimethylolpropane, open the intensification switch of oil bath heater, material in still is heated, when temperature in the kettle is raised to 110 DEG C, add 2 ethyl hexanoic acid and ditrimethylolpropane always to feed intake the 1%(2.35g of quality 235.07g) tosic acid as catalyzer, under nitrogen tube is inserted into liquid level, nitrogen is passed into the flow velocity of 30mL/min, open the stirring of stirrer in magnetic agitation still, timing from now, material in still is warmed up to 190 ± 5 DEG C, heating 21h, the water of observing response by-product is deviate to the speed conditions in collection device under the drive of nitrogen, by the time no longer included after a water deviates from collection device in 10 minutes, sampling,

step S4:the acid number of working sample is 2.8mgKOH/g, because the acid number of sample does not reach≤the level of 1.5mgKOH/g, enters next step;

step S5:continue reaction 1h;

step S6:the reacted acid number of sampling and measuring is 2.4mgKOH/g, due to acid number still > 1.5mgKOH/g, enters next step;

step S7:judge the absolute value of acid number and the adjacent last hypo acid value difference measured in above-mentioned steps S6, due to this absolute value≤0.5mgKOH/g, enter next step;

step S8:due to acid number still > 1.5mgKOH/g, terminate this lab scale, and return step S2, the mol ratio of ditrimethylolpropane and 2 ethyl hexanoic acid is adjusted to 1.04:4, drop into 1.2mol(173.052g) 2 ethyl hexanoic acid, then correspondingly drop into 0.312mol(78.103g) ditrimethylolpropane, all the other process repeats step S3, reaction 21h, sampling, the sample acid number recorded is 1.2mgKOH/g, has reached the requirement of acid number≤1.5mgKOH/g;

step S9:in three-necked bottle, adding ditrimethylolpropane and 2 ethyl hexanoic acid always to feed intake the 1%(2.51g of quality) particle diameter is the gac of 75 μm, continue heated and stirred 1h, then heating is stopped, when being cooled to 60 DEG C in lab scale sample, be carry out suction filtration in the Büchner funnel of the diatomite of 75 μm and middling speed quantitative paper being covered with particle diameter while hot, the product in filter flask is transferred in reagent bottle;

step S10:according to the method that GB/T7305-2003 specify, measure the separation property of synthesis liquid and water, the result recorded is when leaving standstill ten minutes after high-speed stirring terminates, namely the emulsion layer mediated is can't see between oil phase and aqueous phase, namely the volume of emulsion layer is 0mL, represents that the separation property of this synthesis liquid and water is good; The separation property of synthesizing liquid and water due to the result display recorded is good, so need not adjust the mol ratio of this batch of ditrimethylolpropane relative to 2 ethyl hexanoic acid again; Terminate this lab scale, write down this batch of ditrimethylolpropane used and the suitable mol ratio 1.04:4 of 2 ethyl hexanoic acid;

step S11:large-scale production;

Be specially:

Step S111: the suitable mol ratio 1.04:4 adopting the ditrimethylolpropane for present lot and the 2 ethyl hexanoic acid obtained in above-mentioned steps, at 1M ³reactor in, drop into 346.104kg2-thylhexoic acid and 156.206kg ditrimethylolpropane, the total mass of raw material in still is made to reach 502.31kg, open and stir, during beginning, rotating speed maintains 15rpm, open the heating valve of reactor, material in still is heated, when temperature in the kettle is raised to 115 DEG C, add 2 ethyl hexanoic acid and ditrimethylolpropane always to feed intake the 1.0%(5.02kg of quality) tosic acid as catalyzer, open nitrogen valve, nitrogen is passed into the flow velocity of 10L/min, the rotating speed of stirring is brought up to 150rpm, timing from now, material in still is warmed up to 190 ± 5 DEG C, heating 22h, the water of observing response by-product is deviate to the speed conditions in collection device under the drive of nitrogen, by the time no longer included after a water deviates from collection device in 10 minutes, sampling, the acid number of working sample, for 0.95mgKOH/g,

Step S112: because the acid number of sample reaches≤the level of 1.5mgKOH/g, so need not proceed reaction again;

Step S113: add ditrimethylolpropane and 2 ethyl hexanoic acid and always feed intake the 0.5%(2.51kg of quality in reactor) particle diameter is the gac of 75 μm, 0.2%(1.00kg) particle diameter is the diatomite of 75 μm, continue heated and stirred 1.5h, then heating is stopped, when being cooled to 60 DEG C Deng the temperature of product in still, open the valve at the bottom of still, with refining filtering pump by flow out material pumping in pressure filter, order number is adopted to be 270 object filter screens, carry out circulation press filtration, press filtration material out turns back in reactor, after circulation press filtration carries out five minutes, the color of the product returned has not seen that the activated carbon granule of diatomite particle and black remains, product after press filtration being decoloured pours in pail pack.

Adopt aforesaid method to synthesize in the present embodiment and obtain a kind of lurid thick liquid, owing to being adopt ditrimethylolpropane and 2 ethyl hexanoic acid through esterification, and both mol ratio are close to the such theoretical molar proportioning of 1:4, infer so can synthesize corresponding amyl-based polyol fatty acid ester according to the amyl-based polyol adopting in the industry other similar and similar fatty acid ester, the main component of such product should be 2 ethyl hexanoic acid ditrimethylolpropane ester.

Getting the sample of the 2 ethyl hexanoic acid ditrimethylolpropane ester product that above-described embodiment obtains, be placed in reagent bottle, observe under natural light, is lurid thick liquid.Detect above-mentioned sample, recording its kinematic viscosity 40 DEG C time is 158.57mm ²/ s, kinematic viscosity when 100 DEG C is 12.79mm ²/ s, pour point is-17 DEG C, and flash-point is 258 DEG C.

Above content shows and describes ultimate principle of the present invention and principal character.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.

Claims (4)

1. a 2 ethyl hexanoic acid ditrimethylolpropane ester, is characterized in that: its molecular formula is C ₄₄h ₈₂o ₉, there is structural formula as follows: .

2. a preparation method for 2 ethyl hexanoic acid ditrimethylolpropane ester according to claim 1, is characterized in that: the corresponding reaction equation of described preparation technology is as follows:

For ditrimethylolpropane and the 2 ethyl hexanoic acid of purchasing the present lot come, first determine the theoretical molar proportioning of carrying out with 2 ethyl hexanoic acid completely needed for esterification according to the quantity of hydroxyl in ditrimethylolpropane molecule used, or select the mol ratio of current lab scale according to the former experience mol ratio formed for ditrimethylolpropane and 2 ethyl hexanoic acid;

Adopt tosic acid as catalyzer, rely on heating to carry out esterification when logical nitrogen, and the water taken out of with nitrogen is collected by collection device, observe in collection device and no longer included after water deviates from 5 ~ 20 minutes, sampling, the acid number of working sample, makes current lab scale sample meet acid number≤1.5mgKOH/g by the adjustment of one or many lab scale mol ratio;

Add gac, continue heated and stirred 0.5 ~ 2h, then heating is stopped, when being cooled to 50 ~ 70 DEG C in lab scale sample, suction filtration is carried out while hot in the Büchner funnel being covered with diatomite and middling speed quantitative paper, product in filter flask is transferred in reagent bottle, the method specified according to GB/T7305-2003, measure the separation property of synthesis liquid and water; After if the result display high-speed stirring recorded terminates within three ten minutes left standstill after, the volume of emulsion layer is less than 3mL, then represent that the separation property of this synthesis liquid and water is good, terminate this lab scale;

Acid number≤1.5mgKOH/g in this lab scale and synthesis liquid and water separation property also satisfactory lab scale mol ratio carry out large-scale production as the proportioning raw materials of present lot raw material.

3. the method for production 2 ethyl hexanoic acid ditrimethylolpropane ester according to claim 2, is characterized in that described concrete steps are as follows:

step S1: for ditrimethylolpropane and the 2 ethyl hexanoic acid of purchasing the present lot come, the quantity calculating hydroxyl in ditrimethylolpropane molecule used determines the theoretical molar proportioning of carrying out with 2 ethyl hexanoic acid completely needed for esterification, or the mol ratio of current lab scale was selected according to the former experience mol ratio formed for ditrimethylolpropane and 2 ethyl hexanoic acid, the hydroxyl value of a part ditrimethylolpropane is 4, so 2 ethyl hexanoic acid is 4 with the theoretical molar ratio of ditrimethylolpropane;

step S2:the mol ratio setting ditrimethylolpropane and 2 ethyl hexanoic acid in this lab scale is 0.9:4 ~ 1.3:4;

step S3:carry out lab scale, in the three-necked bottle of 500mL, first put into magnetic stir bar, drop into the 2 ethyl hexanoic acid of 0.8 ~ 2.0mol, then the ditrimethylolpropane meeting the respective batch that mol ratio requires in step S2 is dropped into, open the intensification switch of oil bath heater, material in still is heated, when temperature in the kettle is raised to 110 ± 4 DEG C, add 2 ethyl hexanoic acid and ditrimethylolpropane always feed intake quality 0.5 ~ 2% tosic acid as catalyzer, under nitrogen tube is inserted into liquid level, nitrogen is passed into the flow velocity of 10 ~ 100mL/min, open the stirring of stirrer in magnetic agitation still, timing from now, material in still is warmed up to 140 ~ 200 DEG C, heating 10 ~ 24h, the water of observing response by-product is deviate to the speed conditions in collection device under the drive of nitrogen, by the time no longer included after a water deviates from collection device in 5 ~ 20 minutes, sampling,

step S4:the acid number of working sample, if the acid number≤1.5mgKOH/g of sample, then leaps to step S9; If the acid number > 1.5mgKOH/g of sample, then enter next step;

step S5:continue reaction 0.5 ~ 2h;

step S6:the reacted acid number of sampling and measuring, if acid number≤1.5mgKOH/g, then jumps to step S9; If acid number > is 1.5mgKOH/g, then enter next step;

step S7:judge the absolute value of acid number and the adjacent last hypo acid value difference measured in above-mentioned steps S6, if this absolute value > is 0.5mgKOH/g, then return step S5; If this absolute value≤0.5mgKOH/g, then enter next step;

step S8:if acid number is > 1.5mgKOH/g still, then terminate this lab scale, and return step S2, again adjust in the scope of 0.9:4 ~ 1.3:4 and set once the concrete mol ratio of 2 ethyl hexanoic acid and ditrimethylolpropane in lab scale test; If acid number≤1.5mgKOH/g, then enter next step;

step S9:add in three-necked bottle ditrimethylolpropane and 2 ethyl hexanoic acid always feed intake quality 0.5 ~ 2% gac, continue heated and stirred 0.5 ~ 2h, then heating is stopped, when being cooled to 50 ~ 70 DEG C in lab scale sample, in the Büchner funnel being covered with diatomite and middling speed quantitative paper, carry out suction filtration while hot, the product in filter flask is transferred in reagent bottle;

step S10:according to the method that GB/T7305-2003 specify, synthesis liquid in mensuration reagent bottle and the separation property of water, if be less than 3mL at the volume of the three ten minutes internal emulsification layers left standstill after the result display high-speed stirring recorded terminates, then represent that the separation property of this synthesis liquid and water is good, terminate this lab scale, write down this batch of ditrimethylolpropane and the suitable mol ratio of 2 ethyl hexanoic acid, using the mol ratio of this lab scale as proportioning raw materials when carrying out large-scale production with the raw material of present lot; If the separation property of measurement result display synthesis liquid and water is bad, then return step S2 ,in the test of fine setting lab scale, the concrete mol ratio of 2 ethyl hexanoic acid and ditrimethylolpropane, then carries out lab scale next time;

step S11:large-scale production.

4. the method for production 2 ethyl hexanoic acid ditrimethylolpropane ester according to claim 3, is characterized in that the step of described large-scale production is specially:

step S111:the ditrimethylolpropane for present lot obtained with lab scale and the suitable mol ratio of 2 ethyl hexanoic acid, at 1M ³reactor in, drop into 2 ethyl hexanoic acid and ditrimethylolpropane, the total mass of raw material in still is made to be in the scope of 200 ~ 700kg, open and stir, during beginning, rotating speed maintains 5 ~ 50rpm, open the heating valve of reactor, material in still is heated, when temperature in the kettle is raised to 115 ± 5 DEG C, add 2 ethyl hexanoic acid and ditrimethylolpropane always feed intake quality 0.5 ~ 2% tosic acid as catalyzer, open nitrogen valve, nitrogen is passed into the flow velocity of 1 ~ 100L/min, the rotating speed of stirring is brought up to 50 ~ 300rpm, timing from now, material in still is warmed up to 140 ~ 200 DEG C, heating 10 ~ 24h, the water of observing response by-product is deviate to the speed conditions in collection device under the drive of nitrogen, by the time no longer included after a water deviates from collection device in 5 ~ 20 minutes, sampling, the acid number of working sample,

step S112:if the acid number of sample can not reach≤level of 1.5mgKOH/g, then carry out reaction 0.5 ~ 2h, resampling detects acid number, until the acid number≤1.5mgKOH/g of sample;

step S113:add in reactor ditrimethylolpropane and 2 ethyl hexanoic acid always feed intake quality 0.1 ~ 2% gac, the diatomite of 0.1 ~ 1%, continue heated and stirred 0.5 ~ 3h, then heating is stopped, when being cooled to 50 ~ 70 DEG C Deng the temperature of product in still, open the valve at the bottom of still, with refining filtering pump by flow out material pumping in pressure filter, carry out circulation press filtration, press filtration material out turns back in reactor, till the color that circulation press filtration proceeds to the product returned has not seen that the activated carbon granule of diatomite particle and black is residual, product after press filtration being decoloured pours in pail pack.