CN107434775B

CN107434775B - Process for the preparation of liquid phase dialkyl sulfosuccinates

Info

Publication number: CN107434775B
Application number: CN201610586249.4A
Authority: CN
Inventors: 元智援; 金涩基; 林钟峻
Original assignee: Daesung Chemtech Co ltd
Current assignee: Daesung Chemtech Co ltd
Priority date: 2016-05-26
Filing date: 2016-07-22
Publication date: 2020-07-14
Anticipated expiration: 2036-07-22
Also published as: CN107434775A; KR101705868B1

Abstract

The invention discloses a preparation method of liquid-phase dialkyl sulfosuccinate. The method for preparing the liquid-phase dialkyl sulfosuccinate comprises adding 15 to 40 wt% of a dialkyl sulfosuccinate represented by the following chemical formula 1 and 5 to 10 wt% of an antioxidant to 5 to 20 wt% of dimethylacetamide or dimethylformamide, reacting at 75 to 95 ℃, and adding dimethylacetamide or dimethylformamide as a balancing agent to 100 wt%. Chemical formula 1:

wherein R is₁And R₂Are, independently of one another, identical or different hydrogen atoms or alkyl radicals having 1 to 30 carbon atoms, M⁺Is H⁺、Li⁺、Na⁺、K⁺Or NH₄ ⁺A series of cations.

Description

Process for the preparation of liquid phase dialkyl sulfosuccinates

Technical Field

The present invention relates to a method for producing Dialkyl Sulfosuccinate (Dialkyl Sulfosuccinate) in a liquid phase.

Background

In general, dialkyl sulfosuccinates, for example, are added to a polyurethane composition at any point of the composition treatment process when preparing polyurethane fibers, thereby suppressing the generation of static electricity in the product from which the polyurethane fibers are prepared, or providing elastic fibers having excellent adhesion between single fibers.

The dialkyl sulfosuccinate may be added in the form of a solution or slurry in a solution or dispersion of other Polyurethane (PU) or polyurethane fiber additives. They may be mixed with the polymer solution during the treatment process used to make the fibers, or may be injected into the fiber upstream of the last of the spinnerets. Also, the dialkyl sulfosuccinate may be additionally added to the polymer (spinning) solution as a wax or as a solution or suitable for the morphology of the slurry in the medium. In particular, when preparing the usual polyurethanes, the dialkyl sulfosuccinates may be added in the form of the formulations mentioned above.

Also, dialkyl sulfosuccinates may be deposited as terminators when preparing the polyurethane fibers. For example, dialkyl sulfosuccinates may be combined as waxes or in a form suitable for slurry or solution in a solvent in previously known low viscosity polydialkylsiloxanes or mineral oils for the finishing of polyurethane fibers.

Since dialkyl polysiloxanes and dialkyl sulfosuccinates in mineral oils have excellent solubility, a homogeneous solution can be formed, for example, by means of conventional production techniques such as rollers for production or fiber guidance or spraying, and can be deposited on top of the polyurethane fibers.

However, since the dialkyl sulfosuccinate added to the polyurethane fiber requires a purity of 98 or more in terms of reactivity and physical properties, the dialkyl sulfosuccinate is a hard wax-like solid. Therefore, since the dialkyl sulfosuccinate itself has viscosity, inflow of foreign matters, precipitates, and the like may occur in various cases when used in a process, and when used alone, carbonization tends to proceed to a large extent under a condition of a certain temperature or higher.

Disclosure of Invention

It is therefore an object of the present disclosure to provide a method for preparing dialkyl sulfosuccinate in a liquid phase that can solve the above problems.

In order to achieve the above objects, in one embodiment of the present disclosure, a method for preparing a liquid-phase dialkyl sulfosuccinate includes adding 15 to 40 wt% of a dialkyl sulfosuccinate represented by the following chemical formula 1 and 5 to 10 wt% of an antioxidant to 5 to 20 wt% of dimethylacetamide or dimethylformamide, and then reacting the mixture at a temperature of 75 to 95 ℃, and adding dimethylacetamide or dimethylformamide as a balancing agent to 100 wt%.

Chemical formula 1:

According to still another embodiment of the present disclosure, the antioxidant is a phenolic antioxidant.

According to another embodiment of the present disclosure, the phenolic antioxidant is stearyl 3- (3 ', 5' -di-tert-butyl-4 ' -hydroxyphenyl) propionate or tetramethylene-3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate.

According to yet another embodiment of the present disclosure, the reaction is carried out for 4 to 6 hours.

According to still another embodiment of the present disclosure, the method for preparing the liquid-phase dialkyl sulfosuccinate further includes the step of adding 1 to 5 wt% of one or more additives selected from the group consisting of a heat-resistant additive, an ultraviolet absorber, a dyeing property enhancer, and an anti-yellowing agent after the reaction is performed at a temperature of 75 to 95 ℃.

According to still another embodiment of the present disclosure, the heat-resistant additive is triethylene glycol-bis-3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate, or 1, 3, 5-tris (4-tert-butyl-3-hydroxy-2, 6-dimethylbenzene) -1, 3, 5-triazine-2, 4, 6- (1H, 3H, 5H) -trione; the anti-yellowing agent is bis (1, 2, 2, 6, 6-pentamethyl-4-piperidyl) sebacate; the ultraviolet absorbent is 2- (2 ' -hydroxy-3 ', 5' -di-tert-amyl phenyl) benzotriazole; the dyeing property improver is poly (N, N-diethyl-2-aminoethyl methacrylate).

According to still another embodiment of the present disclosure, the reaction is performed under reduced pressure to maintain the moisture content of the final product at 5000ppm or less.

The liquid-phase dialkyl sulfosuccinate prepared according to an embodiment of the present disclosure has relatively excellent heat resistance even when a small amount of an antioxidant and/or a heat-resistant additive is added, so that a carbonization phenomenon does not occur, and thus, when spinning is performed, a precursor (breakage) failure caused by a carbon material is reduced, so that polyurethane fibers can be spun under high temperature conditions, and thus it is very easy to use in a liquid phase, and since filtration is 4 μm or less, when spinning foreign matter, etc., clogging of a filter does not occur.

The features and advantages of the present invention will become more apparent from the following detailed description in conjunction with the accompanying drawings.

Drawings

Fig. 1a is a photograph showing the result of baking dialkyl sulfosuccinate in a liquid phase in an oven at a temperature of 220 c for 4 hours according to a comparative example of the present invention.

Fig. 1b is a graph showing the results of baking a liquid phase dialkyl sulfosuccinate in an oven at a temperature of 220 ℃ for 4 hours according to an embodiment of the present disclosure.

Fig. 2a is a photograph showing the result of dissolving a dialkyl sulfosuccinate at a temperature of 25 ℃ according to a comparative example of the present disclosure.

Fig. 2b is a photograph showing the result of dissolving a dialkyl sulfosuccinate at a temperature of 85 ℃ according to another embodiment of the present disclosure.

Detailed Description

Before describing the present invention in more detail, terms or words used in the specification and the claimed scope of the invention should not be limited to the scope of the general or dictionary meanings, and should be interpreted as meanings and concepts conforming to the technical idea of the present invention on the basis of the principle that the concept of terms can be appropriately defined in order to describe the concept of terms in the best way. Therefore, the structure of the embodiment described in the present specification is only one of the preferred embodiments of the present invention, and does not represent all the technical ideas of the present invention, so that it is understood that various equivalents and modifications that can substitute for these may exist at the time of application of the present invention.

Hereinafter, preferred embodiments of the present invention will be described in detail so that those skilled in the art can easily practice the present invention. Meanwhile, when the present invention is explained, detailed explanations of related art related to the field that unnecessarily obscure the gist of the present invention will be omitted.

As described above, the present invention relates to a method of preparing a dialkyl sulfosuccinate in a liquid phase represented by the following chemical formula 1.

Chemical formula 1:

Dialkyl sulfosuccinates can be prepared as described in the c.r. kary (c.r. carly) literature (ind.eng.chem., vol.31, page 45,1939).

These dialkyl sulfosuccinates are hard waxy solids, and since the dialkyl sulfosuccinates themselves are sticky, they tend to be carbonized to a large extent under conditions of a predetermined temperature or higher when used alone, because they are likely to cause foreign matter, precipitates, and the like to flow into the reactor during the processing.

In particular, preferably, the dialkyl sulfosuccinates are diisobutyl sodium sulfosuccinate, dioctyl sodium sulfosuccinate, dihexyl sodium sulfosuccinate, dipentyl sodium sulfosuccinate, and dicyclohexyl sodium sulfosuccinate. More preferably, the dialkyl sulfosuccinates are dioctyl sodium sulfosuccinate and dihexyl sodium sulfosuccinate. Most preferably, the dialkyl sulfosuccinate is dioctyl sodium sulfosuccinate. Such dialkyl sulfosuccinates may be used as individual substances or as mixtures of a plurality of dialkyl sulfosuccinates.

According to an embodiment of the present invention, the method for preparing the dialkyl sulfosuccinate represented by the above chemical formula 1 as a liquid phase is as follows: adding 15-40 wt% of dialkyl sulfosuccinate and 5-10 wt% of antioxidant to 5-20 wt% of dimethylacetamide or dimethylformamide, reacting at 75-95 ℃, and adding dimethylacetamide or dimethylformamide as a balancing agent to form 100 wt%.

In one specific example, the solvent used in the above method is preferably dimethyl acetamide, dimethyl formamide or the like which is commonly used as a solvent for dialkyl sulfosuccinate, but is not limited thereto, and any solvent having equivalent effects to these solvents can be used.

In the present disclosure, the amount of dimethylacetamide or dimethylformamide is generally about 1.5 to 3 times, or preferably 2 times or more, the amount of dialkylsulfosuccinate in terms of solubility and overall reaction efficiency, which will be described later. In order to obtain a transparent and homogeneous solution, it can be used in 2 steps. The amount used in the 1 st step is 5-20 wt% of the total liquid phase of dialkyl sulfosuccinate, and the amount used in the 2 nd step is determined to form 100 wt% of the balancing agent. In the case where the amount used is less than 5% by weight in the step 1, the dissolving power is reduced to make the final product opaque, and in the case where the amount used is more than 20% by weight, there is a tendency that an opaque product having many suspended matters (high possibility of precipitation) is produced.

According to still another specific example, the antioxidant is preferably a phenol-based antioxidant having a high thermal decomposition temperature, and typical examples of the antioxidant include stearyl 3- (3 ', 5' -di-t-butyl-4 ' -hydroxyphenyl) propionate and tetramethylene-3- (3, 5-di-t-butyl-4-hydroxyphenyl) propionate.

According to another embodiment, the reaction is carried out at a temperature of 75 to 95 ℃, preferably 80 to 90 ℃, or more preferably 80 to 85 ℃ for 4 to 6 hours, or more preferably 80 to 85 ℃ for 5 to 6 hours. If the temperature is less than 75 ℃ or more than 95 ℃, re-agglomeration tends to occur. When the reaction time is less than 4 hours, the undissolved dialkyl sulfosuccinate functions as a seed to be recrystallized, and when the reaction time is more than 6 hours, the dialkyl sulfosuccinate tends to turn yellow.

According to another embodiment, the method may further include the step of adding 1 to 5 wt% of one or more additives selected from the group consisting of a heat-resistant additive, an ultraviolet absorber, a dyeing property improving agent, and an anti-yellowing agent after the reaction is performed at a temperature of 75 to 95 ℃.

Representative examples of the heat-resistant additive include, but are not limited to, triethylene glycol-bis-3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate, and 1, 3, 5-tris (4-tert-butyl-3-hydroxy-2, 6-dimethylbenzene) -1, 3, 5-triazine-2, 4, 6- (1H, 3H, 5H) -trione.

Typical examples of the anti-yellowing agent include bis (1, 2, 2, 6, 6-pentamethyl-4-piperidyl) sebacate, typical examples of the anti-yellowing agent include 2- (2 ' -hydroxy-3 ', 5' -di-t-pentylphenyl) benzotriazole, typical examples of the anti-yellowing agent include poly (N, N-diethyl-2-aminoethyl methacrylate), and typical examples of the anti-yellowing agent include a dye, and suitable additives known to those skilled in the art of the present invention may be used without particular limitation.

Further, according to still another specific example, various stabilizers, i.e., antioxidants such as hindered phenols and sulfur compounds; hindered amine, triazole, benzophenone, benzoate, nickel, and salicyl light stabilizers; molecular weight regulators such as antistatic agents; organic nucleating agents and inorganic nucleating agents; a neutralizing agent; a fluorescent whitening agent; a filler; a flame retardant; and/or flame retardant aids, and the like.

On the other hand, according to another specific example, the reaction is carried out under reduced pressure to maintain the moisture content of the final product at 5000ppm or less. In the case where the dialkyl sulfosuccinate in the liquid phase contains more than 5000ppm of water, such a decompression reaction may cause a phenomenon of lowering the reactivity and performance of the elastomer, thereby making it possible to add a decompression process. Meanwhile, in order to selectively remove foreign materials, that is, dialkyl sulfosuccinate is a product having a viscous solid phase, and thus external dust may flow, it may be filtered using a 2 or 4 micron membrane filter and then used.

Specific examples of the present invention will be described below in more detail with reference to examples, but these examples are only for the purpose of illustrating the present invention and should not be construed as limiting the scope of the present invention.

The measurement method of the physical properties of the polyurethaneurea strand mentioned in the examples and comparative examples described later is as follows.

Strength and elongation:

the measurement was carried out using a tensile tester (UTM, Universal testing machine) made by Instron corporation) at a specimen length of 10cm and a tensile speed of 100 cm/min. At this time, the strength and elongation at rupture were measured, and the load (100%, 300% Modulus) applied to the strand when the strand was 100% stretched and 300% stretched was also measured.

Adsorption force between single fibers:

in a polyurethane elastic yarn formed of a plurality of monofilaments, 1 monofilament is separated into about 5cm, each end of one monofilament and an unseparated monofilament adhered to each other is provided at the center of a 5cm cage so that the intersection point formed by adsorption of the separated monofilament and the unseparated monofilament is located at the center of the 5cm cage, and then the yarn is stretched at a predetermined speed of 1000%/min after being installed in an instron machine equipped with a weighing cell of 1kg or less, thereby measuring the force of one monofilament separated by stretching and the force when the remaining monofilament is separated by stretching. The final value is an average value of values obtained by measuring an average value of the adsorption force exhibited during the stretching, and measuring 5 times or more for each sample.

And (3) testing heat resistance:

the sample was treated in a hot air oven at 200 ℃ for 10 minutes. Before and after the sample was treated, the yellowing value "b" of the sample was measured by a Color-view (Gardener, USA). The difference between the b value after the sample was treated and the b value before the treatment is denoted by Δ b. The smaller Δ b, the slower the yellowing proceeds.

Comparative example 1

7g of dimethylacetamide and 3g of dialkyl sulfosuccinate were mixed for 5 hours at a temperature of about 80 ℃ to obtain a liquid phase of dialkyl sulfosuccinate. The liquid phase of the dialkyl sulfosuccinate is heated in an oven at a temperature of about 220 deg.C for about 4 hours. The result is shown in fig. 1 a. As can be seen from FIG. 1a, it was confirmed that the baked dialkyl sulfosuccinate was considerably carbonized.

Example 1

After 2g of dimethylacetamide and 3g of dialkylsulfosuccinate and 1g of stearyl 3- (3 ', 5' -di-tert-butyl-4 ' -hydroxyphenyl) propionate were mixed at a temperature of about 80 ℃ for about 5 hours, 4g of dimethylacetamide was added to obtain dialkylsulfosuccinate in a liquid phase. The liquid phase dialkyl sulfosuccinate is heated vigorously in an oven at a temperature of about 220 ℃ for about 4 hours. The result is shown in fig. 1 b. As can be seen from fig. 1b, strongly heated dialkyl sulfosuccinates were confirmed to be free of charring.

Comparative example 2

6g of dimethylacetamide and 3g of dialkyl sulfosuccinate and 1g of stearyl 3- (3 ', 5' -di-tert-butyl-4 ' -hydroxyphenyl) propionate were mixed at about 25 ℃ for about 4 hours to obtain a liquid phase of dialkyl sulfosuccinate. After the above liquid phase of dialkyl sulfosuccinate was left to stand at normal temperature for about 4 hours, fig. 2a was obtained. As can be seen from the upper part of fig. 2a, it was visually confirmed that a slight layer separation phenomenon was exhibited as the turbidity of the solution in the container was high. After the liquid-phase dialkyl sulfosuccinate was heated strongly in an oven at a temperature of about 220 ℃ for about 4 hours, it was confirmed from the bottom of fig. 2a that the dialkyl sulfosuccinate was carbonized considerably.

Example 2

After 2g of dimethylacetamide, 3g of dialkylsulfosuccinate and 1g of stearyl 3- (3 ', 5' -di-tert-butyl-4 ' -hydroxyphenyl) propionate were mixed at about 85 ℃ for about 5 hours, 0.2g of triethylene glycol-bis-3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate and 4g of dimethylacetamide were added as heat-resistant additives to obtain a liquid-phase dialkylsulfosuccinate. The above liquid phase dialkyl sulfosuccinate was left to stand for one month under normal temperature conditions, to obtain FIG. 2 b. As can be seen from the top of FIG. 2b, the solution in the container remained transparent. Then, the liquid-phase dialkyl sulfosuccinate was heated strongly in an oven at a temperature of about 220 ℃ for about 4 hours, and finally, as is clear from the bottom of fig. 2b, the dialkyl sulfosuccinate was not carbonized.

Comparative example 3

The polyol was prepared by mixing 2288g of polytetramethylene ether glycol (molecular weight 1815) and 545.625g of 4, 4' -diphenylmethane diisocyanate. A chain extender solution (42.9g of ethylenediamine/13.2 g of 1, 2-diaminopropane: 80/20 mole ratio) was placed in a 2-stage polymerization reactor together with a chain terminator solution (5.25g of diethylamine) and diethylenetriamine as a crosslinking agent.

The amount of diethylamine added was 1/18 (amine equivalent ratio) with respect to the chain extender solution. The amine is placed in an excess of 4 mole percent relative to the equivalents of amine groups to isocyanate groups present in the preliminary polymer. The polymerization reaction is stopped at a point where the unreacted amine content falls below about 4 mole percent. Dimethylacetamide was used as a solvent. As an additive to the solid content of the polymer, 1.0% by weight of triethylene glycol-bis-3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate, 0.5% by weight of 1, 3, 5-tris (4-tert-butyl-3-hydroxy-2, 6-dimethylphenyl) -1, 3, 0.5% by weight of 5-triazine-2, 4, 6- (1H, 3H, 5H), 0.5% by weight of 1, 1, 1 ', 1 ' -tetramethyl-4, 4 ' (methylenedi-p-phenylene) diaminourea, 0.7% by weight of poly (N, N-diethyl-2-aminoethyl methacrylate) as a dyeing property enhancer, and the like were added and mixed, 0.1 weight percent titanium dioxide, to obtain a polyurethaneurea dope.

40daN3 single fiber polyurethane urea elastic yarn was prepared by spinning the dope obtained as described above at a speed of 900m/min by dry spinning (spinning temperature: 250 ℃), and the physical properties thereof were evaluated and shown in table 1.

Comparative example 4

The amount of diethylamine added was 1/18 (amine equivalent ratio) with respect to the chain extender solution. The amine is placed in an excess of 4 mole percent relative to the equivalents of amine groups to isocyanate groups present in the preliminary polymer. The polymerization reaction is stopped at a point where the unreacted amine content falls below about 4 mole percent. Dimethylacetamide was used as a solvent.

As an additive to the solid content of the above-mentioned polymer, 1.0 weight% of triethylene glycol-bis-3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate, 0.5 weight% of 1, 3, 5-tris (4-tert-butyl-3-hydroxy-2, 6-dimethylphenyl) -1, 3, 5-triazine-2, 4, 6- (1H, 3H, 5H), 0.5 weight% of 1, 1, 1 ', 1 ' -tetramethyl-4, 4 ' (methylenedi-p-phenylene) diaminourea, 0.7 weight% of poly (N, N-diethyl-2-aminoethyl methacrylate) as a dyeability improver, 0.1 weight% of titanium dioxide, and the like were added and mixed, 1.0 weight percent of solid phase (waxy) dialkyl sulfosuccinate, to obtain a polyurethaneurea dope.

Polyurethane urea elastic yarns of 40daN3 monofilaments were produced by spinning the dope obtained by the above method at a speed of 900m/min by dry spinning (spinning temperature: 250 ℃), and their physical properties were evaluated as shown in table 1.

Example 3

0.8% by weight of triethylene glycol-bis-3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate, 0.5% by weight of 1, 3, 5-tris (4-tert-butyl-3-hydroxy-2, 6-dimethylbenzene) -1, 3, 5-triazine-2, 4, 6- (1H, 3H, 5H), 0.45% by weight of 1, 1, 1 ', 1 ' -tetramethyl-4, 4 ' (methylenedi-p-phenylene) diaminourea, 0.7% by weight of poly (N, N-diethyl-2-aminoethyl methacrylate) as a specific dyeability improver, 0.1% by weight of titanium dioxide, and the like are added and mixed as additives to the solid content of the polymer, 3.3 weight percent of the dialkyl sulfosuccinate (1 weight percent solids basis) of the liquid phase obtained in example 1, thereby obtaining a polyurethaneurea dope.

TABLE 1

As is apparent from table 1 above, the polyurethaneurea elastomers of comparative examples 3 to 4 and example 3 have excellent or no difference in physical properties such as elongation, strength of 100%, strength of 300%, and adsorption force between single fibers. However, it was confirmed that the polyurethaneurea elastic yarn of example 3 was more excellent in strength and heat resistance (even if a small amount thereof was added, the same effect was actually obtained) than the polyurethaneurea elastic yarns of comparative examples 3 to 4.

Although the present invention has been described in detail with reference to the specific embodiments thereof, it should be understood that the present invention is not limited thereto, but various changes and modifications can be made by one skilled in the art within the technical spirit of the present invention.

The present invention is not limited to the above embodiments, but may be modified within the scope of the present invention.

Claims

1. A method for preparing liquid-phase dialkyl sulfosuccinate, characterized in that after 15-40 wt% of dialkyl sulfosuccinate represented by the following chemical formula 1 and 5-10 wt% of antioxidant are added to 5-20 wt% of dimethylacetamide or dimethylformamide, the reaction is carried out at 75-95 ℃, dimethylacetamide or dimethylformamide is added as a balancing agent to form 100 wt%,

chemical formula 1:

wherein R is₁And R₂Are, independently of one another, identical or different hydrogen atoms or alkyl radicals having 1 to 30 carbon atoms, M⁺Is H⁺、Li⁺、Na⁺、K⁺Or NH₄ ⁺,

Wherein the antioxidant is a phenolic antioxidant.

2. The method of claim 1, wherein the phenolic antioxidant is stearyl 3- (3 ', 5' -di-tert-butyl-4 ' -hydroxyphenyl) propionate or tetramethylene-3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate.

3. The liquid-phase process for producing a dialkyl sulfosuccinate according to claim 1, wherein the reaction is carried out for 4 to 6 hours.

4. The method for preparing a dialkyl sulfosuccinate in a liquid phase according to claim 1, further comprising adding 1 to 5 wt% of one or more additives selected from the group consisting of a heat resistance additive, an ultraviolet absorber, a dyeing property enhancer, and an anti-yellowing agent after the reaction is performed at a temperature of 75 to 95 ℃.

5. The method for preparing dialkyl sulfosuccinate in liquid phase of claim 4, wherein the heat-resistant additive is triethylene glycol-bis-3- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate, or 1, 3, 5-tris (4-tert-butyl-3-hydroxy-2, 6-dimethylbenzene) -1, 3, 5-triazine-2, 4, 6- (1H, 3H, 5H) -trione; the anti-yellowing agent is bis (1, 2, 2, 6, 6-pentamethyl-4-piperidyl) sebacate; the ultraviolet absorbent is 2- (2 ' -hydroxy-3 ', 5' -di-tert-amyl phenyl) benzotriazole; the dyeing property improving agent is poly (N, N-diethyl-2-aminoethyl methacrylate).

6. The method for preparing dialkyl sulfosuccinate in liquid phase according to claim 1, wherein the reaction is carried out under reduced pressure to maintain the moisture content of the final product at 5000ppm or less.